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Oxford EDS AZtec User Manual

1. You can control what overlays you see in the Spectrum viewer via the Confirm Ele ments Settings These overlays can be very useful in helping you to interrogate com plex spectra View Settings Show Markers E Show Peak Shapes E Show Fitted Spectrum E Show No Pulse Pile Up Correction 330 EDS TEM The Business of Science Press Include Exclude once you are satisfied with the identification of each element to build your list of the confirmed elements See Also Confirm Elements Settings Confirm Elements Tools on page 174 Element Lists on page 191 Peak Labels on page 158 Compare Spectra amp MiniQuant Results on page 318 70 Calculate Composition Calculate Composition In this step you can view quant results in more detail using any of the Available Templates To view result select the template that you wish to use Available Templates Spectrum Details Details spectrum Processing Processing Diagnostics Table customizable Single Sp 3352 Quant Result Details Label Element List Type Processing Option Ratio Standard Element Ratio Standard Line Specimen Thickness Specimen Density Automatic Line Selection Thresholding Deconvolution Element Copy Spectrum 2 Current Spectrum f All Elements Silicon K senes 0 nm 0 g cm Enabled Disabled None Ifyou want to see a comprehensive set of results from a single sp
2. For description of each tool see Acquire Spectra Toolbar on page 316 The Compare Spectra amp MiniQuant Results on page 195 option is available in the top right corner of the Spectrum viewer You can compare the current spectrum with any other spec trum from an opened Project on the Data Tree Instant MiniQuant results can be viewed in a table or a bar chart A number of useful shortcut menus are available as right mouse click in the spectrum viewer For details see Context Menus Spectrum Viewer on page 321 Acquire Spectra Settings The settings are described in detail below Energy Range keV Select a spectrum energy range from the available options of Auto 0 10 0 20 or 0 40 keV from the Energy Range drop down list 96 OX sO EDS SEM INSTRUMENTS The Business of Science An appropriate energy range should be selected in conjunction with the current microscope accelerating voltage If the accelerating voltage is above 10 kV in order to view lines which may be excited above 10 keV the 20 keV range should be chosen Below 10 kV it may be more appropriate to choose the 10 keV range since no lines above 10 keV will be excited In the Auto mode the system checks for the accelerating voltage set on the microscope and selects a suitable energy range in the software Number of Channels Select number of channels from the drop down list of Auto 1024 2048 or 4096 4K with which you wish to display the spectr
3. lt e iB EDS TEM The Business of Science This option is used when processing spectra from specimens in which all elements yield X rays which can be readily detected e g steels alloys and other materials with insignificant amounts of elements lighter than sodium e Oxygen by Stoichiometry Use this option if you want the concentration of oxygen to be calculated assuming that it is bound by predefined stoichiometry to all the other analyzable elements The stoichiometry is defined by the valency of the oxygen ions and the valencies of other measured elements Number of Ions Enter the number of oxygen ions that are combined stoichiometrically to the other elements The calculations are based on the number of oxygen ions and how many atoms there are in each unit cell a Valency When Oxygen by Stoichiometry is selected the option for choosing the valency for each ana lyzable element becomes available The most common value for the valency of the element is displayed when you click on an element symbol on the periodic table To use a different value enter the new value in the Valency text box Element List You can select a different type of element list depending on how you want your spec tra spectrum to be quantified e Current Spectrum If this option is selected each spectrum will be quantified using the elements confirmed in the Confirm Elements step for the current spectrum e Fixed List Select t
4. The Business of Science Support Panel The Support Panel is present on the right side of the application window It has three com ponents Data View Mini View and Step Notes You can add or remove any of these com ponents from the display by selecting the View menu on the Menu bar You can also minimize maximize or close each component from the display by pressing the relevant but ton present at the top right corner of each component To increase your work area you may wish to collapse the Support Panel by pressing the arrow button in the top right corner of the application Pressing this again will restore the Support Panel Data View Data View has two tabs one for the Current Site and one for the Data Tree For details see the Data View topic from the link at the end of this topic Mini View In the Mini View you can choose to display a number of different views such as Electron Image Spectrum Monitor the Ratemeter or many others depending on the step Step Notes Step Notes provides the first time user of a navigator with simple instructions on how to com plete a typical work flow It also provides a site administrator or user with the ability to write a standard operating procedure SOP See Also Mini View on page 93 Step Notes on page 94 D7 Data View The Data View panel is located on the right of the main application window By default it is always displayed If it has been taken off the view it can
5. 144 ON INSTRUMENTS The Business of Science Context Menu Item Export Annotations Show Acquisition Areas Details EDS SEM Save As Original Res olution Save As Copy Print Email Settings Show Select All Style Delete Show All Show Selected Show None Show Short Names 145 Acquire Spectra A Acquire spectra In this step you acquire spectra from the current electron image SE BSE You can also recon struct spectra from a Layered Image or X ray map if you have already acquired SmartMaps Real time Compare and instant MiniQuant options are also available here You can display the components that you are working on such as image and spectrum using Eliz ee the controls on this toolbar located in the top right side of the screen You have choice of displaying image and spectrum as shown in the screen shot below or just an image or a spectrum full screen File vew Tehni Tone Help r 9 o Fae i ly Teriba s I zarg r 7 me he feed eT pity k Fene Looe Spectr F START STOF jeie 3 Saecttecorndinmage home SE Electron Image 1 Sprcir tries _ Wit 16 80 rem Inpart Rrte Sit Arps Citar Rather SGA ope Dead Time 25 Penna Tirran 146 EDS SEM 45O ND INSTRUMENTS The Business af Science There is an acquisition toolbar near the top of the workspace Acquire Spectrum gt START STOP settings
6. AutoID E b Clear AI 370 EDS TEM OXF INSTRUMENTS The Business af Science To include an element for mapping either double click on its symbol on the periodic table or click the Include button All the elements selected for mapping are green color coded on the periodic table To exclude an element from being identified by AutoID and excluded from being mapped click on its symbol on the periodic table to select it and then press the Exclude button This element will be removed from the analysis All excluded elements will be red color coded on the periodic table Note An excluded element if present in the specimen may affect the TruMap results To remove an element map from the display select it by clicking on it and then press the Clear button It will be removed from the display Press the Clear All button to remove all maps from the display Remember the maps will be displayed again when you press AutoID or include ele ments manually Manual selection of energy windows and X ray lines Press on the Map Details dialog to open the Selected Elements Details Selected Element Details Element Manganese Label Min Energy Window Selection Automatic Specify Line Series specify Energy Window Lower Energy keV 3 018 Upper Energy keV 5 980 Update A ray map with changes i The default setting is Automatic X ray lines and energy window width selection TO manually define the wi
7. Repeat the previous steps to select further components and complete your tem plate To add an extra page click the Add New Page button which is in the bottom right corner To generate the templates click Generate in the menu bar In the Template Gen eration Options dialog enter the details If you will be the only user of this tem plate select Current User You can create Word and Excel templates Click OK to create the report templates You cannot change the design of these report templates If you intend to change the design of your template later click File gt Save or File gt Save As to create an intermediate XML file at a convenient location Click OK to close the dialog To close the Report Template Generator dialog click X in the top right corner To quickly find your new report template look in your list of favorites Changing an existing report template If you saved your previous design as an intermediate XML file earlier you can open the file again and continue working on your template design 57 L 2 3 4 In the Report Templates dialog click the Template Generator button In the Report Template Generator dialog click File gt Load Using the file browser locate the intermediate XML file and click Open Continue working on your design Getting started The Business of Science Themes There are different themes i e color schemes availab
8. These controls are at the top of the window above the phase maps 233 Description Starts processing the element maps to create each phase map A Cancel button and a progress bar appear during the proc essing Shows the progress of the proc essing For more details hover the cursor over the progress bar for a few seconds Cancel Processing Stops the processing amp Adjusts the settings used dur ing the processing Boundary Tolerance con trols the behavior at the boundaries of each phase The Grouping Level deter mines the numbers of phases that you see See Also Analyze Phases on page 375 Analyze Phases settings on page 381 Finding phases on page 376 Toolbar for Phase Map These controls are at the top left side of the window Moves the image Click the Pan tool then click and drag the image Use the mouse wheel to zoom in and out Normalizes the spectra 234 Oy AE ED EDS SEM INSTRUMENTS Description Adds annotations to the current image The tools include Caliper Angle Text Rectangle and Ellipse Defines points and regions on a map image to extract spectra Shows the energy and counts at any point in the spectrum viewer in the bottom left corner Shows the phase at any point in the phase maps in the top right corner See Also Analyze Phases on page 375 239 Map Custom In the Custom mode the Map navigator has two steps
9. Unlinks images You can manipulate individual layers using pan or zoom controls Use the mouse wheel to zoom in and out of the image Use these tools near the bottom right of the screen to adjust manual and automatic brightness contrast and color Context Menus Right click the electron image to display context menus for copying exporting and printing images See Also Scan Image Toolbar on page 424 Scan Image Settings on page 421 FSD diode controls on page 432 Context Menus Image Viewer on page 157 Export Settings on page 132 AutoLock on page 133 283 Acquire Spectra ccs Acquire Spectra Introduction Having defined the model for your specimen and determined the best conditions kV and X ray lines for analysis aided by using the Simulate Spectra and Set up Solver steps you are ready to acquire spectra from your specimen on the microscope After spectrum acquisition from the current electron image SE BSE of your specimen each spectrum is then quantified in real time These instant quantitative results can be viewed using MiniQuant The real time spectrum compare options are also available to view your results Acquiring Spectra a Set the spectrum acquisition conditions such as kV and X ray lines aided by using the Simulate Spectra and Set up Solver steps or from prior specimen knowledge Performa Beam Measurement using a pure element standard such as Co or Mn in the Calibrate step of
10. 2 0cach0 bsneeiencassetsenasabadnadacemeeseseeagewuass 258 Acquire and Construct Linescans 2 22 259 ODEN ZO Sree raed ceed cee nee eae eee eae dane een neeeen 262 STAVE CZ econ hes a a O ELEA 263 EDS SEM The Business af Science Setup for EDS There are two calibration routines available in the Calibrate step of Optimize navigator Energy Calibration and Beam Measurement To ensure that you understand when to cal ibrate your system and which calibration routine to use read the comprehensive details below Calibrate 2 0 0 0 ccc Loana 66 Calibration Element 2 2 2 2 c ccc ccc ccc cece ccc cece cece ceceeee 70 Calibrate for Beam Measurement Settings 22 71 65 Calibrate Calibrate Two calibration routines available are Energy Calibration and Beam Measurement For qual itative and normalized quantitative analyses you will need to perform only the Energy Cal ibration part However if you are interested in accurate quantitative analysis with un normalized results you will need to perform the Beam Measurement routine too Note You can access the Calibration routines from the Calibrate step in the Optimize navi gator Energy Calibration For accurate identification of peaks you need to perform the Energy Calibration Energy Cal ibration measures the shift in the position of the spectral peaks and resolution of the system As the system has v
11. Counts Linear Logarithmic 107 108 Context Menu Item Normalize Normalize is a useful func tion for com paring two spectra acquired using dif ferent input X ray count rates for example spectra acquired with two dif ferent beam currents Nor malize is available from the toolbar on the left of the screen in Acquire Spectra Con firm Ele ments Acquire amp Confirm and Compare Spectra steps of Point amp ID and Analyzer For details of how to nor malize using a point or a The Business of Science Context Menu Item region ona spectrum see the Com pare Spectra help topic Note that Normalize can be switched on and off from the shortcut menu avail able as right mouse click in the spec trum viewer If a point or region has already been defined on the spec trum switch ing Normalize on or off will maintain the point or region If a point or region has not been defined already switching it on will nor malize the spectra to the peak at zero EDS SEM 109 110 Context Menu Item Smooth This is useful when com paring spec tra where small dif ferences may be obscured by statistical scatter The smooth func tion applies an energy dependent filter to the spectrum This has the effect of slightly broadening the peaks and also fil tering out the rapid fluctuations due to sta tistics Sta tisti
12. D pp j Line Data 1 gt Site3 Add Selected Spectra Spectra Maps Linescans To compare quant results from two spectra select Comparison of Results Two Spectra template Then select the comparison spectrum from the Compare option in the Mini Quant and Compare option The compare spectrum will be overlaid on the current spectrum in the Spectrum Viewer The quant results will be displayed in the table below Ifyou wish to change the Quant Settings press the Settings button to display the Quant Settings dialog Apply the changes and close the dialog Press the Requantify button to display the recalculated results Quant Results Details You can see the settings used for calculating the composition in the Quant Results Details list box Parameter Description Label Spectrum Label E g Soectrum 1 Element List Type Current Spectrum Fixed List or Combined List Processing Options All Elements Element by Difference Com bined Element or Oxygen by Stoichiometry Apply Coating Correction Enabled or Disabled 186 The Business of Science Parameter Coating Element Coating Thickness Coating Density Automatic Line Selection Normalization Thresholding EDS SEM Description E g Carbon E g 15 nm E g 2 25 g cm3 Enabled or Disabled Enabled or Disabled Enabled or Disabled Deconvolution Elements None Selected Factory Standards Standardizations file supplied with the sys te
13. INSTRUMENTS The Business af Science Search Phase St Search Phase This step is divided into three main parts Confirming the presence of elements in your spectrum Setting up the search criteria Conducting the Phase Search Spectrum selection The spectrum displayed in the Spectrum viewer corresponds to the one stored displayed under the currently highlighted Point Data node Highlight a different Point Data node to dis play another Spectrum Alternatively select the required spectrum from the drop down list box positioned above the spectrum viewer this will allow selection of not only spectra acquired from the Acquire Data step but also sum spectra or spectra acquired elsewhere in the application Confirming the elements in your Spectrum Part of this step is designed to help you confirm the elements that have been identified by AutoID in your spectrum The options available are those found in the Confirm element step in the EDS part of the product These elements are then used to create an element list for qualitative and quantitative analysis Note that extensive tools including Element Series Markers Overlays Element Profiles and Show Candidate Elements are available to help you to manually confirm your elements If you wish to manually confirm the automatic peak identification Press the question mark icon to select the Show Candidate Elements tool from the tool bar on the left hand side of the inte
14. Note that Mains Synchronize will only be visible if the appropriate hardware is installed Input Signal Select the signals from the detectors on the microscope 422 EBSD OXF INSTRUMENTS The Business of Science For EDS secondary electron imaging is generally most appropriate if you are imaging a sam ple which has topography whereas backscattered imaging is a very useful means of iden tifying areas of different composition on flat samples Secondary electron imaging is the most common form of imaging and for a first look at your sample choose this mode If you are analyzing a flat polished sample and you can see weak contrast switch to back scattered imaging which will tend to enhance this contrast by showing up areas of different phases For EBSD Forward Scattered Imaging is often used Because of the high angle of tilt dictated by the collection geometry required for EBSD many electrons are scattered forward and down towards the bottom of the phosphor screen Using Forward Scattered Electron FSE imaging diffraction contrast is enhanced and the resultant signal makes the presence of individual grains easy to identify The forward scattered electron signal produced is therefore ideal for EBSD investigations However the user may use any electron signal as required for the reference image If you select the Auto checkbox before you start a new FSE acquisition the software auto matically adjusts the signal from ea
15. OX FORD EDS SEM INSTRUMENTS The Business of Science Ifthe boundary tolerance is low each pixel in the phase represents a pure spec trum If a pixel has contributions from several phases it cannot be identified and appears black Ifthe boundary tolerance is high all pixels are placed in the phase that fits them most closely The spectra for each phase shows small contributions from adjacent phases Low setting of boundary tolerance High setting of boundary tolerance Grouping Level Phase analysis identifies all the phases in the sample Grouping combines phases that are sim ilar and can create a smaller more manageable number of phases overall Ifthe grouping level is low a larger number of phases are displayed The later maps show phases that occupy small areas and might indicate trace compounds Ifthe grouping level is high a smaller number of phases are displayed The maps typ ically show a few large areas 220s If the Grouping Level is too high areas that you consider as separate phases will be merged together To resolve this problem you can reduce the Grouping Level until all the expected phases are shown and then manually merge any phases that you prefer to analyze as a sin gle phase See Also Analyze Phases on page 375 User Profile on page 22 Merging phases on page 379 Analyze Phases toolbars These toolbars are available in the Analyze Phases step Map display tools These contr
16. Show Acquisition Areas in Offers a choice to show any acqui Reports sition areas By default reports show none Package Templates Offers a choice of templates for each package A report is a Microsoft document or spreadsheet in one of several page sizes Letter is popular in the USA The default paper size A4 is popular in Europe Other Templates Offers a choice of templates for the batch export of data Status Bar You can select the parameters such as microscope voltage and noise levels for EDS and EBSD that will appear in the Status Bar at the bottom of the software window Welcome Screen You can choose whether the Welcome Screen appears when you start the software The Wel come screen shows a list from which you can quickly select any of your recent projects See also Status Bar 19 Status Bar The Status Bar displays the hardware status It also allows the access to the Microscope Con trol EDS detector and EBSD detector A progress bar appears in the Status bar when you import load or save projects The user selected parameters are displayed in the Status Bar at the bottom of main appli cation screen You can choose the parameters you wish to display on the Status Bar tab in the Preferences dialog To access the Preferences dialog go to the Tools menu on the main tool bar and select Preferences Preferences Auto Save m z E AAAA AAAA Bo Parameter Current value EBSD 3D Phase
17. The default peak labeling behavior is controlled by the User Profile You can access the User Profile screen from the Tools menu on the main application window Select the Peak Labels tab from the User Profile screen Profile ESS 0 Camere Schra Lib leet LOS LP Fher Se etn Seething 1 2 Fiare rater PAS TP Soker Seine Ehrat emi amp inc a oe pee E Perec rare ERD Spodra Oe ral Sees BUG riogqeure Lire Lia Stree TO fever hlapi orien Lierrean erpin ED ding oe Speeds a Tai co bres lu Llasct Bord um EDS Earm icip E E biladi ira LES Peak Label Settings m x TA E kalt i a E 1 i FGETS bel Jaani eri ae EDS TEH Quart Shige oan Irae Debir eer mi E opt rey Hewmt A Hermen rmt Dereenk You can select how you wish to display labels on the peaks from the following three options 158 EDS SEM Oy 45O ND INSTRUMENTS The Business af Science 1 Element Symbols e g Mn 2 Element Symbol amp Line e g Mn Kal 3 Element name e g Manganese Make your selection by checking the relevant radio button This configuration is saved with the User Profile Note that peaks will be labeled according to your new selection on the next spectrum acquisition The labels on the current spectrum will not be automatically updated To update the labels on an existing spectrum use the Apply Profile button on the Confirm Elements step shown in the screen shots later on in this topic When you
18. To delete annotation click it to select it Press the Delete key on the keyboard or use the context menu to delete the annotation EBSD Tool Description Positions the beam Click the tool then click on the image to position the beam around the image and check the quality of the EBSPs from different points on the spec imen The EBSP appears in the top right quad rant unprocessed EBSP You can control the beam by the mouse Alternatively you can use the arrow keys on the keyboard Then you can use the Shift key for a coarse shift and Ctrl for a fine shift The On Off and Center buttons are linked with this tool If you click On the tool is auto matically selected Shows the intensity and beam position for any pixel in the image Click the tool and then hover on the image The values appear as you move from pixel to pixel 443 Optimize Solver Optimize Sober This step contains the necessary functions to allow you to acquire index and refine EBSPs Positioning the Beam As you enter this step the Acquire an EBSP from a point tool is selected by default When this tool is selected the beam can be positioned on the image and its position can be con trolled by the mouse as well as by the keyboard Shift will give a coarse shift and Ctrl will give a fine shift Note that you can also center the beam by pressing the Center button Once the beam is positioned release the mou
19. selecting elements for mapping You can access Map Details option from s located at the bottom of the workspace 219 v Map Details i Eg i A m A m A af La AutolD K b tear Al a To include an element for mapping either double click on its symbol on the periodic table or click the Include button All the elements selected for mapping are green color coded on the periodic table To exclude an element from being identified by AutoID and excluded from being mapped click on its symbol on the periodic table to select it and then press the Exclude button This element will be removed from the analysis All excluded elements will be red color coded on the periodic table Note An excluded element if present in the specimen may affect the TruMap results To remove an element map from the display select it by clicking on it and then press the Clear button It will be removed from the display Press the Clear All button to remove all maps from the display Remember the maps will be displayed again when you press AutoID or include ele ments manually Manual selection of energy windows and X ray lines Press on the Map Details dialog to open the Selected Elements Details 220 EDS SEM OXF INSTRUMENTS The Business of Science l Selected Element Details Element Manganese Label Min Energy Window Selection Automatic Specify Line Sen pecify Line Senes Specify Energy Window
20. 189 Selecting an element for deconvolution means the peaks will automatically be deconvolved from the spectrum but the element will normally not be quantified The deconvolution ele ment will only be quantified if its composition is entered as fixed wt or is calculated by stoi chiometry or difference Threshold Quantitative Results Quantitative results are displayed with value which is one sigma standard deviation based on counting statistics Typically results which are less than 3 sigma have reduced sig nificance and so it may be desirable to set them to zero Thresholding may be applied so that results below the selected sigmas are set to zero Thresholding will also ensure that negative insignificant values which sometimes result from trace element analysis are set to zero To enable Threshold Quantitative Results check this option in the Quant Settings The default value for Sigma is 3 which represents 99 7 confidence level Quant Standardizations The system is supplied with factory standardizations To use your own standards for quan titative analysis you first need to acquire spectra from standards and perform at least one standardization using the Standardize step on the Optimize navigator When you have done this your user file will be available to select for use by the User radio button under Quant standardizations in EDS Quant Settings If the Factory button is selected factory stand ardizations will be u
21. Binning combines a group of pixels into one new pixel The binning appears to shorten the linescan at each end In the following example with a binning factor of 16 the first value appears at approximately 8 um because the first binned point is midway between the first 16 values 224 OXKOIRD EDS SEM INSTRUMENTS The Business of Science 12000 E 12000 10000 9000 a000 aC 00 2 e000 7000 i lar il ERT EE ili BETER l nil ERTER l IIN 6000 6000 5000 5000 a 5 3 00 2000 z a haw a a Mean imams E L T Pan Sey cas EE I 8 12 16 20 24 28 32 36 40 paral pk ct pet tel fl ae cod eet a ede ick a maj 0 4 8 1 16 20 24 28 32 36 40 Original data at 1 um spacing Binned data 229 Analyze Phases In this step the software automatically converts X ray maps into phase maps The phase maps help you to see the constituent elements of the phase and how the phases are dis tributed over the specimen The window has several sections Element map Individual phase maps and the elec tron image Combined phase map image gt Minimized phase maps Phase Details Spectrum The individual phase maps top right are presented according to the distribution and size of each phase The first maps show large areas of closely grouped ele ments Later maps show smaller areas that are more finely distribut
22. Context menu Right click on the EBSP to access various options in the context menu such as blinking the solution and removing the display of detected bands It is also possible to switch on off the display of the Pattern Center marked with a green cross Further options are available under Preferences from the main menu Status bar beneath the EBSP Cycle Times Two cycle times are shown below the EBSP The Analysis time is the time it takes for the soft ware to perform the analysis of the acquired EBSP and the Detector time is the time it takes for one EBSP to be acquired by the detector and transferred to the PC The Analysis time will depend on the selected analysis parameters and the Detector time will depend on the selected detector settings In order to acquire data at high speed it is impor tant to keep both the Analysis time and the Detector time low If the analysis time is highest then the system will acquire at a lower speed than indicated by the detector time Number of Bands This is the number of bands detected on the EBSP Band Contrast Band contrast is an EBSP quality number The higher the number the better the EBSP quality Band Slope Band slope is an EBSP quality number The higher the number the better the EBSP quality 445 Hough Viewer The Hough space display accessed by pressing X shows the EBSP after transformation into Hough space The Hough transformation converts Kikuchi bands into peaks which a
23. Data from Map Acquisition The Data Tree gets populated with the new items as data is being acquired as shown in the screen shot below 207 Electron image Data View leone It can be a secondary electron image at ee SE backscatter electron image BSE z Em or a forward scattered electron image a a Specimen 1 _ Appropriate detector hardware needs rA Site 1 9 be etane L eu can also import an image into the Project _ Electron Image 1 S Map Data Map Data 1 M EDS Data The EDS and EBSD Map data are con a Spect tained in the Map Data folder The EDS R ae Data folder contains Map Sum Spec Mg Kal Z trum and X ray Element Maps Ti Kol Cr Kal Mn Kal X ray Element Maps Two modes of mapping are available Window Integral Maps and TruMaps EDS Layered Image 1 To select the mapping mode press the Map Data 7 Map or TruMap button above the map BEDS Data display Standard Window Integral maps counts in the energy window are acquired for the element list chosen Ti Kal for analysis These are raw X ray maps Cr Kal which are not corrected for back Mn Kal ground or peak overlaps Map Sum Spectrum Mg Kal _2 a r EDS Layered Image 2 Second mode of mapping is TruMap You can process the map data as Tru Maps which are corrected for back ground and peak overlaps Mineral im ported image EDS Layered Image It is a composite image generated by overlaying selected X ray m
24. Electron Image 1 Display Stacker Settings Line Data 6 ia ie rly 50 f a l ess ERN 2 imm om Minimised Lines Mode _ on The progress of line data acquisition is displayed in Current Site tab in the Data View 4 Element linescans start to populate the Linescan viewer as the data is being acquired 5 You can stop the acquisition by pressing or the red STOP Button To cancel the line processing click the Cancel Processing button in the acquisition tool bar 6 From the controls above the Linescan viewer choose how to process the data for example TruLine 391 The TruLine data processing will use the TruLine settings from the EDS Element settings tab in the User Profile screen You can access the User Profile from the Tools menu You can specifically define whether the threshold is on by selecting Apply threshold for TruLine and entering a Sigma Threshold between 0 0 and 3 0 See Also User Profile on page 22 Acquire Line Data Settings on page 252 392 gt EDS TEM OXF INSTRUMENTS The Business of Science Displaying and manipulating linescans Three different views are available from the controls in the top right corner of the Acquire Line Data screen Display Electron Image Full Screen Display Linescans and Electron Image s Display Linescans Full Screen Ole se Several options are available to view the Linescans a Stacked multiple linescans overlaid are d
25. ID Navigator in the Custom mode It is aimed for users who do not require any guidance during their analyses The workspace is divided into four quadrants Each quadrant represents an application For example Scan Image is located in the top left quadrant Acquire Spectra in the top right quadrant Quant Results in the bot tom left quadrant and Confirm Elements in the bottom right quadrant Press the relevant button in the toolbar from the view in any quadrant To re dock the free floating window back into the main application window press Ea Each application has identical functionality as its counterpart in the Guided Navigator To get help on each application follow the links below Scan Image on page 418 Acquire Spectra on page 350 Confirm Elements on page 353 Calculate Composition on page 185 20Ls Recommended way of working in Point amp ID Custom Mode In the Custom mode four smart components are available in one window You can acquire review confirm and process data in one window You do not need to move away from it dur ing the analysis The four smart components are docked in the workspace as the default layout Each com ponent can be un docked and have it as a free floating window It can be resized and dragged to a second monitor to be viewed in full screen There is a great deal of flexibility in the user interface to customize the layout to suit your requirements EXAMPLE One way of working in the Cus
26. Save To Profile EEE Clearall EDS SEM O 45O ND INSTRUMENTS The Business of Science Peak Labels Lines to label Manganese LI 0556 keV Lr 0567 keV 636 keV 0 649 keV 3 586 keV 5 899 keV 6 491 keV s Apply Profile f Save To Profile The lines which are checked are the ones used for labeling the peaks in the current spectrum You can check or uncheck a line to add or remove the label To save your labeling con a Save to Profile e button after check figuration for an element in the User Profile press the ing the lines Apply Profile To use the labeling configuration saved in the User profile press the button This action will remove all labels from the current spectrum and apply labels according to the scheme saved in the User Profile Moving Peak Labels Manually Click on the peak label that you wish to move and drag it to a new position by holding the left mouse button After moving the peak labels on the current spectrum you can restore them to their original position by selecting Reset Positions from the Peak Labels section of the context menu on the Spectrum viewer Notes Ifthere are too many labels too close together only main peak labels are displayed The hidden labels will reappear if you stretch the spectrum along the x axis You may find that previously hidden labels show up when labels are moved or deleted a All existing pea
27. See Also NanoAnalysis Encyclopedia for Pole figures and Inverse pole figures 470 ON5 OND INSTRUMENTS The Business of Science Export Settings on page 132 Preferences on page 13 Context Menus Pole Figure and Inverse Pole Figure Tab below Context Menus Pole Figure and Inverse Pole Figure Tab A number of useful shortcut menus are available when you right click on the Pole Figure tab and it is displaying a pole figure or inverse pole figure Menu option Description Settings Opens the Settings dialog so that you can change the phase or direction Select Projection Type Offers a choice of the type of projection equal area or ster eographic When you select this display setting it is applied to all your inverse pole figures You can also select this option on the Preferences dialog on the Pole Figure tab Select Symbol Size Offers choices of the pixel size Nor mally one scatter point is represented by only one pixel if you select Large each point is represent by many more pixels making smaller features easier to see Draw Great Circles Shows the latitude and longitude lines on the sphere When you select this dis play setting it is applied to all your pole figures for Pole Figure only You can also select this option on the Preferences dialog on the Pole Figure tab 471 Menu option Description Overlay on Sphere Shows the location of the inverse pole figure
28. The sigma values are displayed as black or white vertical bands across the bars in the chart results as shown in the example above In this case the full scale of the bar chart is 50 If you wish to change the MiniQuant Settings press Ed All Elements Spectrum 1 Oxygen by Stoichiometry Spectrum 2 e Fe Element by Difference EB Normalize Results Apply Br oy Weight Make your selection by clicking on the radio button and then press the Apply button The results will be updated immediately Note The Quant Settings in the MiniQuant and Calculate Composition are the same Updat ing one updates the other and vice versa 114 EDS SEM Oy 45O ND INSTRUMENTS The Business of Science Confirm Elements ontinm Elements This step has been designed to help you confirm the elements that have been identified by AutolID in your spectrum These elements are then used to create a confirmed elements list for qualitative and quantitative analyses Extensive tools including Element Series Markers Overlays Element Profiles and Show Candidate Elements are available here to assist you in confirming elements manually How to confirm elements Start with the largest peaks Press the question mark icon to select the Show Can didate Elements tool from the tool bar on the left hand side of the interface then double click on a peak in the spectrum viewer The candidate elements are dis
29. co s tit anton dant cee daun ot 0000000000000000 oaeo ononon noone nonnene 241 Displaying and manipulating linescans 0 222 c cee eee eee cece ee eee ee eee 243 Measuring the distance between two points 000 2c cee eee eee cece ee eee eee 245 Viewing element counts and percentages 2 222 cece cece ee eee ee eee ee eee ee 246 Comparing element quantities 0 0 020 e ee cece eee eee eee 247 Smoothing the linescans 00 22 e cece cece eee eee eee eee eee e eens eeeee 248 Hoes ar lee ane eret oe ara a a OE eet PY eee OT 249 Exporting the linescan data 0 00 22 c cece eee cece eee eee eee eee ee eee 250 Extracting a single spectrum from the linescan 2 22 2 eee eee cece eee eee ee 251 Extracting multiple spectra from the linescan 0 2 2 0 e cece eee cece ee eee eee 252 COMMS ERO CE LUNES CAN Ssh osc er AE ESAE EE 255 UTI Si ANNE SUIS COIN Saat foe fara te heehee tna ates treads Ni eee Rn N eR eatin tat 258 Contents The Business of Science Acquire and Construct LineScans 2 0 00 2 eee eee eee cece cece eee ee eens 259 OBI Ze E E ET EA iceescecseeetendsteceeusesereneceeesscaees 262 Standardize aoaaa aa aaao ca 0000000000000000 a000 teed dee alceeeneetecenseneaiatceanese 263 Ee dad 0 0000000000000000 00000000000 000000000000 n ienee noain inne nr nnn nnennnnn 270 LayerProODE oeocroicenrr eaea EE EEE EEEE 271 Describe SpeciMen sossrosisssdisrsrcscrdot
30. option you need to enter the element symbol followed by weight e g for FeS2 it will be Fe 46 55 S 53 45 It will be symbol weight symbol weight until you have added all elements The total weight has to be between 95 and 105 If it falls outside this range you will be warned about it Standards Standards are materials which are used to relate the intensity of a peak in a spectrum to the concentration of that element in the specimen They are materials in which the concentrations of all the elements are accurately known Standards may be pure ele ments or compounds High quality reference standards are essential to perform accu rate quantitative microanalysis in the SEM Not only must their chemical composition be well characterized but they must also be microscopically homogeneous stable under the electron beam and prepared with a flat polished surface How to standardize 266 Ensure that the spectrum to be used for standardization is displayed in the spec trum viewer This may be a spectrum you have just acquired in either the Analyzer or in Point amp ID or you may wish to standardize using a stored spectrum Select the standards block you wish to use from the Block drop down list in the Standards Composition section Select the standard that you wish to use from the Standard drop down list If you wish to set up a Deconvolution element select it and add it to the Deconvolution text box Select either Pure Element
31. ratio that is obtained is then multiplied by a pixel whose value is mid range Note that division is used because the strength of the pattern signal correlates with the variation in the back ground There are two methods commonly used when applying a background correction Static and Dynamic A static background is a model of the background generated by averaging a large number of pattern images based on the signal from many different orientations A dynamic background is a model of the background extracted from and used on the same pattern image It can be derived by fitting a suitable mathematical model of the background to the image or by filtering out the high frequency pattern tak ing the low frequency residual as the background Static background In order to use a Static background press the Collect button and select the number of frames A higher number of frames will give cleaner EBSPs but will take longer to collect Note that the default value is 64 frames You are then able to use the Static background correction by checking this option 438 EBSD The Business of Science The simplest way to define a background is to rapidly scan an area of the specimen that con tains many grains and while acquiring an average EBSP Backgrounds for single crystals may be produced by heavily defocusing the electron beam on the specimen Advantages A static background can compensate for sensitivity variatio
32. run after all the map data has been acquired and elements have been identified 1 In the acquisition toolbar click the green Find Phases button to start processing When processing is finished phase map data appears on the Data Tree for exam I Ti 2 AlMgO 2 AIMgO 3 FeMincr 2 Tore run the processing with different settings select the Settings cog icon from the top toolbar Any changed settings are retained in your User Profile and become your default settings when you next run this analysis 3 After the processing you can manipulate the phases as required Examine the spectrum at any point or area on the phase using the tools in the left toolbar to confirm the composition Select individual phase maps to include in the combined phase map You can also include the electron image Merge phases that you want to analyze as a single phase Remove phases that are not relevant to your analysis Rename the phase maps in the Data Tree to identify possibly significant phases For example rename CaSiO to Calcium Metasilicate Change the color of phases for convenient identification See Also Analyze Phases toolbars on page 383 About phase maps The name of each phase is derived from its main elements For example a phase with the fol lowing spectrum might be named 2 FeTiO Although the spectrum contains Si and Al the s221 quantities are much smaller and therefore those elements are no
33. sition parameters Input Count Rate cps Output Count Rate cps Dead Time Ratemeter also displays the current Process Time and the Recommended WD mm Step Notes Step Notes provide the first time user of a navigator with simple instructions on how to com plete a typical work flow It also provides a site administrator or user with the ability to write an SOP Standard operating procedure 94 EDS SEM Oy 45O ND INSTRUMENTS The Business of Science A default editable set of notes are provided for each navigator step The user can then over write these or add notes as required A reset to default settings is available The notes are saved with the current user profile See Also Step Notes Editor on page 43 95 Acquire Spectra at Acquire spectra Analyzer is microscope centric application You can acquire a spectrum from a region on the specimen scanned by the electron beam There is an acquisition toolbar near the top of the workspace It has controls for starting and stopping the spectrum acquisition There is a Settings cog for selecting the acquisition parameters For details see Acquire Spec tra Settings on page 313 The toolbar located on the left side of the workspace has various tools for spectrum manip ulation and annotation as shown in the screen shot below Tools to pan normalize add annotations and show data values Drop downs with alternative options
34. structed during or after data acquisition Generating a Layered Image or X ray maps can bea very useful way to find out what is going on in your specimen EXAMPLE I want to know where certain key elements are distributed over a defect Once I have this information I can determine what caused the defect and advise my production department How to Acquire and Manipulate Maps There are two different types of maps that you can acquire Window Integral Maps or Tru Maps Historically Window Integral Maps have been the standard mode for X ray maps These are ideal when there are no overlapping peaks and you are not looking for trace elements in your specimen The second mode of mapping is with TruMaps which are ideal for specimen containing ele ments with overlapping peaks and removes false variations due to X ray background You can easily switch between the two modes of mapping during acquisition by pressing the Map or TruMap button above the map display Select the acquisition parameters from the Settings cog on the acquisition toolbar gt START and press to acquire map data from the full frame TO acquire maps froma region select a map acquisition tool from Rectangle Ellipse and Freehand tools available from the toolbar 205 206 Tools to pan normalize and add annotations Drop downs with alternative options Tools to specify rectangular elliptical and freehand regions on an electron image
35. 2 AIMgO x 2 AIMgO 3 FeMntCr To re run the processing with different settings select the Settings cog icon from the top toolbar Any changed settings are retained in your User Profile and become your default settings when you next run this analysis After the processing you can manipulate the phases as required Examine the spectrum at any point or area on the phase using the tools in the left toolbar to confirm the composition Select individual phase maps to include in the combined phase map You can also include the electron image Merge phases that you want to analyze as a single phase Remove phases that are not relevant to your analysis Rename the phase maps in the Data Tree to identify possibly significant phases For example rename CaSiO to Calcium Metasilicate Change the color of phases for convenient identification Analyze Phases toolbars on page 383 376 EDS TEM OXF INSTRUMENTS The Business of Science About phase maps The name of each phase is derived from its main elements For example a phase with the fol lowing spectrum might be named 2 FeTiO Although the spectrum contains Si and Al the quantities are much smaller and therefore those elements are not included in the phase name Piper pepepeperperpeprepeprpepepepeprpreprepugey 0 10 keV The names of the cations and anions are arranged in an order that closely resembles the name of a chemical compound The name of the ph
36. 222 0222 c eee eee cece ec ee ec ceeecceeees 444 Acquire Map Data 2 02 2202 c cece eee eee ec eeeeee 450 Construct Maps 0 0022 2 463 Phase i D 2 8 08 cee cee cee cece cee cece ceeeteeseeeseeees 473 Acquire Data 2 2 222 c eee e cece cece ec cceccecceeeeee 474 Search Phase 2 22 2 cece cece cece cece eee eecceeseeeeeees 477 Identify Phase 20 2 02222 eee cece eee eee e cece eeeeee eee 480 EBSD 411 412 Describe Specimen 00000000000000000000 0000000000000 00000000M 413 Scan Image mesecs aaa a a S 418 Optimize Pattern 000000000000000000 0000000000000000 00000000M 436 Optimize SOV OR aca 5 ees saws ede 0000000000000000 000000000 444 Acquire Map Data 0 000 020 2 o cece cece eee cee eee eee 450 Construct Maps 0 00 022 2 cece cece ee ee eee 463 EBSD Oy 45O ND INSTRUMENTS The Business af Science Describe Specimen e Describe Specimen In this step you can record information about your specimen such as its coating and view phase information Summary In the Summary view you can write notes on the project and the specimen within the project For convenience you can also copy images or diagrams and text from other documents or email and paste into these windows Notes are saved with the Project and you can edit notes in any step of the Navigator The notes help you to capture the important information du
37. 223 How binning affects the quality of your data on the facing page solas OXF EDS TEM INSTRUMENTS The Business of science How binning affects the quality of your data As the electron beam scans a line or area of the specimen data is acquired from numerous points Inevitably the signal from each point includes some noise If data is not acquired for long enough the noise level will be high By combining signals from several neighboring points the binning technique produces an averaged signal which has less noise overall The effect is similar to collecting the original data at a lower resolution and a longer dwell time You can select the binning factor from the drop down list below the map or linescan display Effect of binning on element maps A binning factor of four combines 16 adjacent pixels from each 4x4 square into one new pixel For example Binning is useful when you are using the TruMap mode for mapping because of the improved statistics Binning also enables AutoLayer to combine similar maps more suc cessfully because of the lower noise See also AutoLayer on page 222 Effect of binning on linescans Binning combines a group of pixels into one new pixel The binning appears to shorten the linescan at each end In the following example with a binning factor of 16 the first value 3 3 appears at approximately 8 um because the first binned point is midway between the first 16 values 1
38. 243 Thickness in Pixels In addition you can change the color and thickness of individual lines from the Settings in the Linescan viewer toolbar 244 EDS SEM OXFORD INSTRUMENTS The Business af Science Measuring the distance between two points The distance between two points in the Linescan viewer can be measured using the Caliper tool 1 Select the tool from the toolbar on the left and move the mouse over a Linescan viewer stacked or tiled This cursor will track the mouse movement 2 Double click to set the first measurement point 3 Move the mouse to paint a region on the viewer which shows the distance between the two points This will update as the second cursor is moved 4 Double click to fix the position of the second cursor Bevel pa ee RR 900 1000 100 1700 1300 NOTE Unlike calipers on an image the linescan calipers are not saved with the data When you switch to a different tool the caliper information will disappear and will not reappear when you switch back A new region can be drawn by double clicking in the viewer at the new start point You can then define the extent of the measurement by placing the sec ond marker as described above To get rid of the region on the viewer you should switch to another tool on the toolbar In the Vertical Tiles view you can use the Caliper tool on individual linescans to display the dis tance between two points 245
39. All subsequent reports will display your new logo If the Report Template dialog is currently open and your new logo does not appear immediately click Refresh List and wait a few sec onds Generating your own report template Although the software includes a comprehensive list of report templates you might some times need to create a new report template The Report Template Generator allows you to design a new report template and publish it for personal use or to be shared with other users You can use the new template straightaway for producing Microsoft Word and Excel reports You can also save the template in an intermediate form which allows you to con tinue to update the template design over time To create a report template spi 10 11 12 13 In the Report Templates dialog click the Template Generator button In the Report Template Generator dialog enter a title for your template To ensure that you can easily find your template later specify its properties by select ing the technique category paper size and orientation Under Components select the information that will appear in your report For exam ple to add the date go to General and click Date which has this icon to denote it as a piece of text An area appears on the white page Move your cursor onto the page then move or stretch the area as required You can also delete any unwanted component For a context menu right click the area
40. Context Menu Item Reset Scales Export Peak Labels Annotations Save AS EMSA Copy Print Email Settings Show Reset Posi tions Show Select All Style Delete Show s321 22 Context Menu Item Locked This is a useful option if you are looking for a particular energy range You do not want the energy scale to change when you load a new spectrum In the viewer for exam Ination or for report ing Locking the X Axis will main tain the hor izontal energy scale If you do not lock it it will change to the full scale when you load a different spectrum The default energy range Is full scale Adjust EDS TEM The Business of Science Menu Item Show Locked 323 324 Context Menu Item Units You cps eV have the choice between cps eV per channel and Counts for the units along the Y Axis of the spectrum For easy comparison of spectra cps eV is an ideal choice because there is very small var lation in the range You do not need to nor malize prior to com parison of spectra using dif ferent energy ranges number of channels and live times This is vital when comparing a stored spectrum with one that is still EDS TEM The Business of Science Menu Item acquiring Counts Linear Logarithmic 32 326 Context Menu Item Normalize Normalize is a us
41. Current Spectrum Current Spectrum Ad docx EDS TEM Analyzer Template Current Spectrum Current Spectrum Atdod EBSD Phase ID Template Electron Image EBSD Point Electron Image PointAcquireA4 docx EBSD Map Template Electron Image EBSD Maps Electron Image EBSD Maps A4 docx Image Viewer INCA Image Export Welcome Screen Other Templates Batch Template Electron Image Multiple Spectra Electron Image Multiple Spectra A4 docx The resolution of images in your reports can be specified by setting the Dots per Inch DPI option You can specify whether the area selections are shown in the Electron Images The Report Preferences also allow you to specify which Report Template is associated with Batch Reporting mode This is useful for generating similar reports for many sites Generating similar reports for many sites The software has a Batch reporting feature which allows you to generate similar reports from any number of sites For example you can generate a report containing only electron images and spectra from every site Decide which report template to use for generating your batch report You need to do this only once For example you want reports of spectra always to be Word documents for print ing later in Letter size 49 1 On the Tools menu select Preferences and then select the Reports tab 2 On the Reports tab under Batch Report select a suitable template for example Image amp Sp
42. Data is the container for Map Sum Spectrum Reconstructed Spectra X ray element maps and Phase Images Map Sum Spectrum The sum spectrum is calculated from the data acquired from all the pixels in the electron image Reconstructed Spectrum You can reconstruct spectra from regions of maps or linescans X ray Element Maps 88 EDS SEM OXF INSTRUMENTS The Business af Science The data can be processed as Windows Integral Maps or TruMaps FLS maps The Data Tree is populated with the appropriate maps on selection of the map processing option Windows Integral Maps The standard element maps obtained from the counts in the element energy window includ ing the background TruMap The maps are corrected for peak overlaps and any false variations due to X ray background 4 lt gt Sitel _ Electron Image 1 Map Data 1 WY EDS Data Map Sum Spectrum Be Kal_2 Mo Lal Ti teal Phase Image Phase Image is the container for all the phase maps and their spectra For example An image of an individual phase The name is composed of its elements for example AIMgO 1 Ti 2 AlMgO 2 AIMgO pN A spectrum extracted from all the mm points in a phase 3 FeMntr Layered Image Layered Image is a composite image created from electron and X ray map images 89 Linescan Data The data tree contains a Line item under the Site this is the container for the line data By default this
43. EXAMPLE My company has several sites all over the world performing similar types of analysis We need to ensure that each site carries out the same type of analysis in the same way so we can compare results I need some help interpreting recently acquired data if I send a project to Oxford Instruments Customer Support how do I ensure that they see what I do For both these cases the user profile can be exported via the user profile window Save User Profile Please select a profile from the list or enter a new name below Current Settings Application 1 steel Analysis Profile Name Steel Analysis The profile will be saved as a config file and there will be user standards file with ois exten sion if selected for use See Managing Standardizations on page 267 22 Both files must be given to the person who you want to repeat or look at your data The recip ient will have to go to the Load Profile window and import the supplied profile EXAMPLE For spectrum acquisition you can specify the Number of Channels Energy Range keV Process Time Acquisition Mode and Acquisition Time s and save them in the User Profile When the User Profile dialog is opened it stores the backup copy of the current settings Load Press load in the User Profile dialog to load a profile in the User Profile dialog to save a profile Press Press in the User Profile dialog to save the settings T
44. Global Menu Bar There is a Menu bar near the top of the application window It has the common menu items that you can access wherever you are in the application EXAMPLE File View Techniques Tools Help Configurable Status Bar The Status Bar is located at the bottom of the application window You can choose which hardware parameters you wish to display in there A progress bar also shows up in the Status bar when you are importing or saving a project Tool Bars Various useful tools are available in local tool bars where appropriate EXAMPLE Pan Normalize Annotations Show Data Values and Show Candidate Elements tools are available in a local tool bar in the Confirm Elements and in the INSTRUMENTS CX HOR Getting started The Business of Science Acquire amp Confirm windows in Point amp ID on the right of the application window EXAMPLE This tool bar is available in the Acquire and Confirm window in the Custom Map navigator You can toggle on off the user interface components from the display to your preferred layout Context Menus Many useful menu items are available on the right click of the mouse in the application EXAMPLE Image Spectrum and Map viewers have many useful menu items For example you can email a spectrum image or map or append it to your report There are two modes of operation Guided and Custom Guided Mode The user interface components are laid out in Nav
45. Microsoft Word format You can also change the default report template from the Tools menu by changing it in the Report Preferences Report Preferences The preferences used for generating reports are accessed via the Tools menu on the main application screen Select Preferences and then select the Reports tab Preferences allow you to specify how your images will look in your final reports and which Report Template is asso ciated with each navigator The following dialog shows a typical choice of report templates Your list of reports might be different because of the products that are installed Ag Getting started OXFORD INSTRUMENTS The Business of Science Preferences Auto Save Report Image Scaling Pixels Per Inch EBSD 3D Phase Viewer Show Acquistion Areas in Reports Show All EBSD Pole Figure Viewer Show Selected Show None EBSD Image Viewer EDS Layered Image Settings EDS Linescan Viewer Package Templates EDS Spectrum Viewer EDS SEM Point amp ID Template Layer Map Layer Map A4 xlsx EDS TEM Point amp ID Template Electron Image Spectrum Electron Image Spectrum A4 docx Reports EDS SEM Map Template Status Bar Maps L Maps A4 L docx EDS TEM Map Template Maps L Maps A4 L docx EDS SEM Linescan Template Linescan Tied Linescan Tiled A4 docx EDS TEM Linescan Template Linescan Tiled Linescan Tiled Ad docx EDS SEM Analyzer Template
46. Save As Ongin Mergi Enport Data Orily Save Aa Print Etil Deiml Settings panels a Settings panels can now behave in two different ways depending on the users pref erence Stay open until the cog or cross is pressed Stay open until a mouse click anywhere on the interface STOP H Settings Select Second Image None 3DE E Scan Image Settings Image Capture Image Scan Size 1024 Dwell Time us 1 Input Signal EF SE E BSE E Software Tilt Correction E Continuous Scan Interface reset Once activated the interface layout will go back to default X View Techniques Tools Help Data View Mint View Step Notes Applicaton Zoom Level Reset Layout kV visible on Mini View Mini View Ratemeter Input Count Rate 0 cps Output Count Rate 0 cps Dead Time 0 Process Time 4 Recommended WD 25 0 mm High Voltage 20 0 kV EDS usability improvements and new functionality Noise Peak Option to Include Exclude the noise peak in the scaling of the spec trum You can hide the noise peak if you do not wish to display it in the spectrum Reset scales Export Peak Labels Annotations X Aas Y Axis Nonmalize Smooth Noise Peak Indude in Scaling Exclude from Scaling v Hide Details See the link below for details X What s New in Version 2 0 Oy 45O ND INSTRUMENTS The Business af Science Context Me
47. Stage Tilt 414 EBSD OXF INSTRUMENTS The Business of Science The Stage tilt value is automatically read from the microscope via the Microscope Control However if this value is not automatically read you may enter the value in the Microscope Control window Total Specimen Tilt This value is the sum of the Stage tilt and the angle of the Pretilted holder This is the tilt angle which is being used by the software for analysis so check that the specimen tilt is cor rect before doing any experiments This can also be shown in the Status Bar and is shown by default Specimen Orientation In the Specimen Orientation tab it is possible to define a data rotation which is saved with the Project The data shown in the application is always the original unrotated data so the selection in the Specimen Orientation tab does not affect the way the data is displayed however it works as a placeholder for saving information about the Specimen Orientation If a rotation trans formation is saved with the data then the cpr file after export to CHANNELS format will also contain information about this rotation so that data viewed in the CSO coordinate system Sample Primary Coordinate system will be shown with the saved rotation Once the data Is exported it can also be rotated from CHANNELS s Virtual Chamber tool and this tool can also be used to alter any rotation saved from the software The six buttons shown are associated with
48. The Business af Science Inthe map display settings you can sort maps alphabetically by atomic number or by maximum map intensity You can also smooth maps by choosing the smoothing level from the Settings Using the Auto Brightness and Gamma buttons on the bottom right hand corner of the Map display window allows you to change the Bright ness Contrast and Gamma for all the maps The Auto Brightness button optimizes the maps to give the best Layered Image and the Auto Gamma enables you to see all the map data including background noise You can choose the color for your maps adjust intensities and decide which maps to add to the Layered image Alternatively you can let the software do this auto matically Pressing the AutoLayer button which is located in the bottom right hand corner of the Map Display window will automatically scale and color all the maps and select the best ones to provide an effective color image that delin eates regions of different composition Maps will be auto brightness corrected and those that show similar structure will be assigned the same color Maps that are very noisy will be shown in grey The most significant map for each assigned color will be added to the Layered Image See AutoLayer on page 222 for detailed infor mation If your data contains a lot of noise binning might help you to achieve a better Auto Layer result Select the binning factor from the drop down list below the maps
49. The Describe Specimen step is covered in the earlier section The step which is unique to this navigator is described here Acquire and Construct 2 222 022 oe e cece eee eee ee ec eeeeeeee 237 236 EDS SEM The Business af Science Acquire and Construct Acquire and Construct Scan Image Acquire Map Data and Construct Maps are laid out as separate steps in the Guided mode of the Map application There are four components that make up these three steps an Image window an X ray map window a Spectrum reconstruction window and a Confirm elements window These four components are combined in the Custom mode to give you a single workspace called Acquire and Construct It offers the convenience of working in one window without having to move away from it The user interface components are docked in the workspace in the four quadrants Each com ponent can be undocked in a free floating window It can be dragged on to another monitor resized or displayed in the full screen view There is a toolbar located near the top right corner of the workspace with icons which allow you to toggle on off each component The user interface elements are described below Electron Image Layered Image The Scan Image component is docked in the top left quadrant It allows you to acquire an electron image and a Layered image You can choose to display either the electron image or the Layered Image Press ass to acquire or disp
50. Ti Lower Energy keV Upper Energy keV Update ray map with changes l The default setting is Automatic X ray lines and energy window width selection To manually define the width of the energy window select the Specify Energy Win dow option Enter the values for Lower Energy keV and Upper Energy keV and a Update X ray map with changes b l The map will be acquired using the defined press window width To manually select the X ray line for mapping an element select the Specify Line Series option Select the line from the Line Series drop down list and press a Update X ray map with changes I a E The map will be acquired using the specified X ray line Reconstruct spectra from Layered Image or Maps using Point Rectangle Ellipse and Freehand tools The spectrum reconstruction tools are available in the toolbar on the left of the workspace Select the spectrum reconstruction tool from the four available options Tools to specify points and regions on an image for spectrum reconstruction 221 a Click on any image and drag with the left mouse to select a region A reconstructed spectrum is displayed in the spectrum viewer and it is also added to the data tree MiniQuant results of the reconstructed spectrum are displayed You can compare the sum spectrum and the reconstructed spectra To confirm the elemental composition of a phase you can navigate t
51. When the run starts if there are not enough measurements to determine a suitable interval use either the minimum allowed user specifiable interval currently 5 141 seconds or use the frame time for the tracking image whichever is larger If Pre dictive Drift Correction is enabled this limit will be either the predictive reference interval or the frame time whichever is larger Start accumulating drift in pixels Once two reference images have been collected the accumulated drift over time is determined AZtec then determines if drift exceeds the target max drift value in pix els the target max drift is 1 5 pixels Assuming the target max drift has not been exceeded the system will estimate when that target will be reached and the next measurement interval is scheduled for this point If the target max drift has been exceeded the system will estimate when that target was reached and use this to determine the measurement interval We also reset our accumulated drift to zero and restart the associated timer The same limits apply to the automatic measurement as are in place for the values which can be manually entered currently 5 seconds to 30 minutes For Predictive Drift Correction the minimum time is at least as big as the predictive reference inter What is In Field Mode In this mode the entire scanned area i e field of view is always viewed The tracking image used is equivalent to a 2x zoom image from
52. X ray element maps and Phase Images Le Map Sum Spectrum The sum spectrum is calculated from the data acquired from all the pixels in the electron image w Reconstructed Spectrum You can reconstruct spectra from regions of maps or linescans X ray Element Maps The data can be processed as Windows Integral Maps or TruMaps FLS maps The Data Tree is populated with the appropriate maps on selection of the map processing option Windows Integral Maps The standard element maps obtained from the counts in the element energy window includ ing the background TruMap The maps are corrected for peak overlaps and any false variations due to X ray background 4 gt Sitel Electron Image 1 Map Data 1 Wy EDS Data Map Sum Spectrum Be Kal_ Mo Lal Ti Kal Phase Image 293 Phase Image is the container for all the phase maps and their spectra For example An image of an individual phase The name is composed of its elements for example AIMgO 1 Ti 2 AlMgO 2 AIMgO A spectrum extracted from all the m points in a phase 3 FeMinCr Layered Image Layered Image is a composite image created from electron and X ray map images Linescan Data The data tree contains a Line item under the Site this is the container for the line data By default this is labeled as Line where is an auto increasing number under the current site Site 1 as shown below Project 1 a Specim
53. Yes Sodium K senes Albite m Sodium Ksenes Albite n i Magnesium i senes MgO P Magnesium series MgQ j Silicon senes S102 a Silicon senes S102 Phosphorus K series GaP Yes Phosphorus K seres GaP Yes Sulfur K senes Fe5z Yes Sulfur K senes Fe52 Yes Chlorine K seres NaCl Yes Chlorine K seres NaCl Yes l Argon K seres Ar v Yes Argon Ksenes Ar v Yes l Potassium K senes KBr Yes Potassium Ksenes KBr Yes Calcium K senes Wollastonite Yes Calcium K seres Wollastonite Yes Scandium Ksenes Sc Yes Scandium Ksenes Sc Yes Titanium Ksenes Ti Yes l Titanium K series Ti Yes Vanadium Ksenes W ne Vanadium Ksenes V ym Chromium senes Cr Chromium j senes Cr CETHE es Manganese es Iron Fe Tron senes Fe 268 EDS SEM The Business af Science Press the Copy button to copy the selected entries Sharing standardization files You can share standardization files with other users of the system by using the Export and Import options available in the User Profile dialog from the EDS Quant Setting tab Select User Profile from the Tools menu Select EDS Quant Settings in the User Profile dialog Select the Standardization file from the Quant Standardizations Press the Save As button The Save User Profile dialog is displayed Enter the name for the User Profile or select an existing User Profile from the list in the Save User Profile dialog Press the Export butt
54. a large number of offline PCs Network licences are designed for offline processing on multiple PCs Requires installation of the AZtec software on the individual PCs and on the user s local network server All installations on a single server need to be the same package i e Standard Advanced Automate Users on a PC connected to the local network server run the AZtec software locally and it automatically communicates with the server to see if any licences are avail able If a license is available the AZtec software runs as normal If all licenses have been checked out the user receives a notification and has to contact the local administrator The local administrator is notified when available licenses are running low The Network license also allows users to check out an available license for use away from the local server network This timed license deactivates when the period has elapsed and returns to the local server for re use Note CHANNELS still requires a HASP dongle yi What s New in AZtec 2 1 Oy 45O ND INSTRUMENTS The Business af Science Interface modifications and GUI usability improvements AZtec has anew welcome screen that allows Quick access to recent projects Quick access to demonstration data for training purposes Quick access to Help Creation of a new project with an associated profile The Map and TruMap icons have been modified and moved closer to
55. a line spectrum over the current spectrum The MiniQuant results are displayed in a table as shown in the example below 181 Spectrum 1 Spectrum 2 Wt o WW o Fe Ti The results are displayed as wt weight The statistical error is displayed as weight sigma for the calculated wt It is the overall confidence figure for the analysis You can use sigma to assess the results especially when an element is present at low concentration For example if an element concentration is 0 2 wt and the is 0 12 wt the element might be detected at a statistically significant level if the acquisition time for the spectrum is extended If the is 0 4 wt it is pointless to extend the acquisition time and it is safe to assume that the element if present is at a level above the limit of detection for this technique Press to display the results in a chart Spectrum 1 Spectrum 2 The sigma values are displayed as black or white vertical bands across the bars in the chart results as shown in the example above In this case the full scale of the bar chart is 50 If you wish to change the MiniQuant Settings press Ed 182 EDS SEM OXF INSTRUMENTS The Business of Science All Elements Spectrum 1 Fe Element by Difference EB Normalize Results Apply Make your selection by clicking on the radio button and then press the Apply button The results will be updated imm
56. are defined in the Quant Settings dialog which is available in the User Profile and the Calculate Composition window Note that the Fixed List is only used for calculating composition in quantitative analysis Example I want to do quantitative analysis on my glass samples and want to compare results from one batch to another batch I am always looking for the same specified list of ele ments You can specify the Element List for Quant from the three available options in the Quant Set tings dialog as shown in the screen shot below 193 Element list E E casera Select an Element list for the Fixed List ae quantitative analysis from Fixed List and Current Spectrum the three options Iron Element Quant Line Fixed Weight Iron Titanium Fe and Ti are selected as the Fixed List elements but you can overide the choice if required Add element Remove element Clear all elements Element List Quant Element List Details Current Spectrum This list includes the Pre defined Elements and elements identified by Auto ID and manually using the Candidate Element tool Fixed List You select the Fixed List option if you know what elements you wish to quantify Choose the elements from the drop down list as shown in the screen shot above Fixed List and Current Spectrum To quantify the elements in the above two lists select the Fixed List and Current Spectrum option MiniQuant results table will c
57. are hidden in the Auto mode Custom In the Custom mode you can define all AutoLock settings including Tracking Image Scan Set tings and Predictive Correction as shown in the screen shot below 134 EDS SEM ON INSTRUMENTS The Business of Science AutoLock Settings CHT Auto Custom Tracking Image image scan Sipe 25 Dwell Time iust 10 Frame Time secs 05 Input Signal SE Scan Settings W Use Automatic Measurement Interval AuutoLock Mock In feld Fxtenched filet Maximum Drift of held Width 50 Gx zoom Use Predictive Conection Reference Interval secs 10 2 Start image acquisition by pressing the Start button It will initialize the AutoLock and then acquire an electron image The AutoLock Settings can only be changed if no data has been captured for a given electron image in this case an existing elec tron image will be deleted and replaced unless you have locked the image in the Data Tree Note If data has already been collected changing the AutoLock Settings will require start ing a new Site During data acquisition you can choose to display the status history and diagnostic infor mation of AutoLock in the Mini View AutoLock Progression The drift profile is shown as snail trail yellow It represents the amount of drift that has occurred The full dark area around the image represents the total imaging area if a full 100 scan was captured T
58. as very high values to the left of the his togram maybe 100 across 1 2 pixels For less stable samples the histogram will spread to the right 136 EDS SEM Oy 45O ND INSTRUMENTS The Business af Science In the worst case the histogram will show large peaks to the right hand side indicating that large amounts of drift have been detected In this case you may want to stop the sample and take corrective action Very large drift values will be clamped to the right side of the histogram once they get beyond a certain value The cut off point will be based on the AutoLock Settings The histogram will reset for each acquisition i e it will only show the drift from the current acquisition You can export the raw drift values times and distances as a CSV file via the context menu on the Mini View AutoLock Information The following diagnostic data is displayed if you select AutoLock Information in the Mini View Mini View AutoLock Informaton Active Cornection AutoLock Status Drift Proximity 6 Selected Item Last Drift Correction pixels 4 52 Max Drift Correction pixels 8 58 Last Dnft Correction nmi 11288 99 Max Dnft Correction nm 21437 59 Active Correction AutoLock Status and Drift Proximity are displayed here AutoLock Status The current status is displayed here 137 Drift Proximity The remaining drift range as a percentage of the field width
59. be present You define your Fixed List using the Periodic Table as described in bullet number 2 above The Confirmed Elements List is from the Current Spectrum This list includes all the elements identified by AutoID and any other ele ments that may have been added to the Confirmed Element list manually What elements are quantified when you select Fixed List and Current Spectrum are shown in the examples below in a table Fixed List Current Spectrum Combined List Spectrum 1 Si O Si O Al Ca Si O Al Ca Spectrum 2 Si O B N Si O B N Quant Element List Details From this tab you can view the details of each element in the list The default setting is that the X ray lines to be used for Quant are automatically selected You can manually select the X ray line for each element if you un check the Automatic selection of line for all elements option You can check the Fixed weight option and enter the value Deconvolution Elements Deconvolution elements may be used to select elements present in the spectrum that should not be quantified but whose influence needs to be accounted for when processing the spec tral data For example elements present in an oxidation layer or in a substrate layer If you wish to deconvolve elements from a spectrum select the required element from the drop down list and press Add element Further elements can be added or removed using Add element or Remove element respectively
60. be restored by choosing the Data View from the View menu on the main menu bar Data is archived in a logical manner and can be directly viewed via easily recognizable icons Acquired data is automatically saved at the end of an acquisition An auto save option can be enabled from the Auto Save tab of the Preferences on page 13 dialog on the Tools menu The Data View panel has two tabs Current Site and Data Tree See Also Current Site on the facing page Data Tree on page 85 28 Getting started Oy 45O ND INSTRUMENTS The Business af Science Current Site The Current Site shows the data for the currently selected Site in the Data Tree plus the cur rent acquisition and any pending acquisitions The ordering of items in the Current Site is dif ferent to the Data Tree The new data items are added to the end in the Current Site where as the Data Tree sorts the items under the Site by spectra electron images and then maps The Current Site has some extra features Electron Image Electron image has a lock unlock icon Click once to lock then again to unlock Electron Image 1 oO Electron Image 1 Oo If unlocked subsequent electron image acquisitions in the same Site will replace the existing electron image Locking the Electron Image will prevent the image from being recycled Current Acquisition Both Spectrum and Map acquisitions show a progress bar and a stop icon spectrum fj When acquir
61. been specified these will be included for identifying and labeling peaks in the current spectrum automatically Note that the Identified Elements are saved in the Spectrum Perform Auto ID During Acquisition option is enabled by default and can be deactivate by un checking it in the Describe Specimen step as shown in the screen shot above You can then AutoID at any time by pressing the button 192 OXFORD en INSTRUMENTS The Business of Science Additional peaks in the spectrum can be identified manually by using the Show Candidate Elements tool in the Confirm Element step Click on the question mark icon to select the Show Candidate Element tool Position the cursor at the center of a peak by double clicking with the mouse The list of elements spectra corresponding to the energy at the cursor is dis played in the panel on the right By highlighting an element in this list you will see the markers showing all the lines for this element Note that the Identified Elements will be quantified if you have selected the Current Spec trum or the Fixed List and Current Spectrum Element List in the Quant Settings in the Cal culate Composition step or EDS Quant Settings in the User Profile dialog Note EDS Quant Settings are available in the User Profile Dialog accessed from the Tools menu These settings are also available from the Calculate Composition step Fixed List The elements in the Fixed List
62. before user data acquisition begins This method of drift correction is typically used when acquiring EBSD data as it typically suits the type of drift seen when analyzing tilted samples Why does AZtec only require 2 image scans for Predictive Drift Correction when Fast Acquisition required at least 3 The predictive algorithm in AZtec is different from Fast Acquisition and as such we only need two images However there might be gains to be made in increasing the initial predictive ref erence interval times What Is the Measurement Interval The measurement interval is the time in seconds between the tracking images Drift cor rection is applied after each tracking image is collected For small amounts of drift a longer measurement interval is sufficient If the sample drifts a lot then shorter measurements are required for accurate data collection The default value is 30 seconds What is the Automatic Measurement Interval AMI If the Automatic Measurement Interval is selected then the system will determine a suitable measurement interval for you This interval is adaptive so if the rate of drift changes so will the drift interval This option will work with both predictive and reactive drift This measurement interval is determined based on a maximum target drift between corrections and this maximum is 1 5 pixels How is the Automatic Measurement Interval AMI Set The automatic drift is calculated in the following way a
63. both EDS and EBSD data simultaneously Goto the Search Phases step to confirm the elements present by selecting the spectra and or map sum spectrum in the spectrum viewer Set the phase search criteria to generate the candidate phase list 466 EBSD The Business of Science Go to the Identify Phase step to index the EBSP using the list of candidate elements generated The EBSP should index with a good fit and an acceptable MAD value Select the best solution and click Add Phase for Acquisition Go to the Optimize Solver step to acquire an EBSP froma point on the map If Auto is selected in the processed EBSP quadrant the software will automatically snap detect and index the EBSP Go to settings and change desired number of bands Hough resolution etc and the solution will be updated Alternatively you can manually click index after each setting is changed Please note that you if you are interested in saving a pattern and solution you will need to use the Extract an EBSP from a point Bloons The extracted point data will be saved under an Extracted Point Data node in the data tree Reanalysis of a Complete Map Go to the Construct Maps step when your map with stored patterns has been collected or highlight your chosen map in the Data Tree Optimize any acquisition settings i e phases Hough resolution number of bands and number of reflectors However note that you can not change the step size to this
64. click on an element symbol on the Periodic table a list of X ray lines together with their energies is displayed This list corresponds to those in the X ray database The lines which are checked are the ones used that will be used for labeling peaks You can check or uncheck a line to select or deselect it for labeling To restore the settings to the factory set ses tort tings for this element press the button You may have configured lines for other elements To restore them to the factory settings a Reset All Elements i press the button This action will restore all the elements to the default settings Refining Peak Labels Manually You can manually refine the peak labels for an existing spectrum in the Confirm Elements step You can configure which lines you wish to be labeled for each element from the Peak Labels tab or Peak Labels slide out menu as shown the screen shots below 159 Confirm Elements Settings a Candidate Elements ay Spectrum 5 Mn profile z 150 Se p AN l Si 2 Manganese Mn Kal i B 100 gt a 3 Promethium Pm LB1 50 od CC prnni Ped Ph eue Le Ge L 0 4 6 keV Chromium CrkB1 Periodic Table Element List Peak Labels Lines to label Manganese E 0 556 keV Ei Ln 0 567 keV E Lal 0 636 keV E g1 0 649 keV T pray Holmium Ho L i i E Apply Profile
65. coating The adjusted value will be used in the quant calculations Quantification During quantification for a coated specimen corrections will be made for the reduction in the effec tive kV for the primary beam when entering the specimen and the reduction in the emergent X ray intensity due to the additional absorption of the coating layer Thus for a particular specimen the values of the concentrations will increase when the coating correction is enabled and in general the effect will be most pronounced in the case of spectra acquired at low kV Coating Techniques Unless you are working with a variable pressure or low vacuum microscope it is important that the sample you are analyzing conducts sufficiently so that it does not charge under the electron beam It also may not be a problem if you are using very low voltages There are a number of ways to reduce charging including coating your sample with a conductive material prior to obser vation in the SEM Coatings are usually applied by using a vacuum evaporator or a sputtering device For X ray microanalysis we recommend that you use carbon since it does not generally interfere with elements of interest in the sample Gold usually used when a good secondary elec tron image is required is not recommended for X ray microanalysis because of the large number of lines in the gold X ray spectrum which may overlap with the lines of interest from your sample Evaporation The most common for
66. collect The time per frame displayed under the histogram includes the frame aver aging 439 Please note that there is a slight difference between the frame averaging that is applied to the live monitoring of EBSPs and the frame averaging that is applied when snapping an EBSP or doing mapping The frame averaging method for monitoring uses a rolling average buffer so that the view can be refreshed at the rate of the camera Other EBSP acquisitions will col lect precisely the number of frames from the camera as specified in the Frame Averaging setting for each beam position and average those frames together to form a single proc essed EBSP Magnetic Field Correction This section is available only if this feature has been licensed and activated To setup the cor rection click Setup and use the dialog that appears To apply the correction select the check box If the correction has been applied to maps or patterns it is indicated in their details See Also Optimize Pattern Toolbar on page 442 Context Menus Image Viewer on page 157 Brightness Contrast and Gamma Controls on page 214 Magnetic Field Correction Setup below Magnetic Field Correction Setup This window is launched from the Optimize Pattern step A correction factor is calculated which will subsequently be applied to all distorted EBSPs if enabled A pair of distorted and undistorted EBSPs need to be collected Fromas near the same place as pract
67. confidence figure for the analysis You can use sigma to assess the results especially when an element is present at low concentration For example if an element concentration is 0 2 wt and the ais 0 12 wt the element might be detected at a statistically significant level if the acquisition time for the spectrum is extended If the a is 0 4 wt it is pointless to extend the acquisition time and it is safe to assume that the element if present is at a level above the limit of detection for this technique Press Ga to display the results in a chart Spectrum 1 Spectrum 2 Br Weight o The sigma values are displayed as black or white vertical bands across the bars in the chart results as shown in the example above In this case the full scale of the bar chart is 50 If you wish to change the MiniQuant Settings press Ed All Bements Spectrum 2 Oxygen by Stoichiometry Spectrum 1 Thickness nm 0 00 Density g cm 0 00 Apply Weight Make your selection by clicking on the radio button and then press the Apply button The results will be updated immediately 320 The Business of Science Note EDS TEM The Quant Settings in the MiniQuant and Calculate Composition are the same Updat ing one updates the other and vice versa Context Menus Spectrum Viewer A number of useful shortcut menus available as right mouse click in the spectrum viewer are shown in the table below
68. down list Choose the spectrum acquisition parameters from the Settings cog For details see Beam Measurement Settings Get the element standard in the field of view of the microscope Adjust the working distance to the recommended value and the beam current to achieve an optimum count rate Press to start acquisition of the calibration spectrum The current set tings will be used to acquire the spectrum A window will be painted across the peaks of the element X ray line series A progress bar near the top of the Calibrate window displays the estimated time for the completion of Beam Measurement routine The progress is also displayed in the Current Site tab of Data View in the Support Panel On completion of the Beam Measurement routine a message is displayed to save it if you wish If you decide to save it the calibration spectrum Is saved in your Project Note that the details of Beam Measurement can be found in the Spectrum Details dialog in the Calculate Composition step when a spectrum has been quantified See also Calibration Element on next page Calibrate for Beam Measurement Settings on page 71 69 Calibration Element Select the element that you wish to use for calibration from the drop down list The choice of element depends on whether you are doing Energy Calibration or Beam Measurement For Energy Calibration The elements available for Energy Calibration are tabulated below X ra
69. ee eeeeeee 387 386 EDS TEM The Business af Science Acquire and Construct Acquire and Construct Scan Image Acquire Map Data and Construct Maps are laid out as separate steps in the Guided mode of the Map application There are four components that make up these three steps an Image window an X ray map window a Spectrum reconstruction window and a Confirm elements window These four components are combined in the Custom mode to give you a single workspace called Acquire and Construct It offers the convenience of working in one window without having to move away from it The user interface components are docked in the workspace in the four quadrants Each com ponent can be undocked in a free floating window It can be dragged on to another monitor resized or displayed in the full screen view There is a toolbar located near the top right corner of the workspace with icons which allow you to toggle on off each component The user interface elements are described below Electron Image Layered Image The Scan Image component is docked in the top left quadrant It allows you to acquire an electron image and a Layered image You can choose to display either the electron image or the Layered Image Press ass to acquire or display the electron image Press to acquire map data or dis play the Layered Image Element Maps The Element Maps component is docked in the top right quadrant of the Acquire and Con st
70. elements you can produce a Microsoft Word or Excel report You can email the spectrum to your customer directly from the spec trum viewer provided your system is connected to the network and it has appropriate soft ware installed You can use the confirmed elements list for elemental maps and quantitative analysis Below is step by step guide for qualitative analysis to get the most accurate results out of your system with minimal effort Ifyou know what elements are present in your specimen and you only want to see peak labels or X ray maps or X ray linescans for those elements then you can select them in the Pre defined Elements tab in the Describe Specimen step of Point amp ID Map or Linescan navigator Ifyou are interested in seeing what other elements might be present then select the AutoID option by checking the Perform AutoID During Acquisition check box Note Check the EDS Element Settings in the User Profile dialog available from the Tools menu to ensure that the elements that you have pre defined in the Describe Spec imen step are not in the Exclusion Elements List Users can have different exclusion lists Acquire an electron image from an area on your specimen in the Scan Image step available in the Point amp ID Map and Linescan navigators Navigate to the Acquire Spectra step Press to acquire a spectrum from the entire image If you wish to acquire a spectrum from a point or an area on the im
71. esensi r EE EERDE 406 Acquire and Construct LineScans 2 000 222 cece eee eee eee eee cece ee eee ees 407 EBSD na nee me ta a Soe een Rt BO Ee eNO Cae Re RE etree OEE et RAT Fe 411 BO Ie Din oi Ws eet ios eee eo de ee tet Nee eek Sede eae a 412 DESCHIDE SPECIMEN aaisen 22a Sa caaialds a boadouties feats ese anoeraag secede 413 SGA Ue O Chet es tnd ees ka cecus ees ate ates a at AOE 418 XX Contents The Business af Science Optimize Pattern 0 2 2 0 cece ce cee cece cece cece cece ee ceeeceeeceeeseeeeuees 436 Optimize Solver 0 02 cece ccc e cece ee cece cece cece cceeeceeeeceeecceueceeeeeeeenes 444 Acquire Map Data ede ban cecet auc as nero ae eedeene es ase asieccoes ee ceeneseeeweseee 450 Construct Maps 2 eee cee cee cee cece cece cece cece eee cee cece ceeeceeeceeeeees 463 PRS Does eis eee ee eee eee a E E 473 Acquire Data ice ccanscessesteunnssadesdubdasccwnddecdemeseneucecddeueddousseceesseccesweaes 474 Search PAS ss sets eee eed ade eee E OERA EATE E 477 Identify Phase 00 0 0 2 cee cece cece cece eee ee eee e cece cece eee e ee eeeeeeeeeeees 480 Hardware Control 1 22 0 eee eee eee eee e eee eeeee 483 Detector Control 2 22 eee eee cece eee eee eeeeeees 484 EBSD Detector Control 0 000 22 o cece cece ce cee ee eee eee ee annona 489 Microscope Control 2 222 222 c cece c eee c cece cece cece cece cece eee ceeeeceeeeeeeeeeeeeees 493 Microscope Parameters
72. for map acquisition Tools to specify points and regions on an image for spectrum reconstruction Tool to show data values on an image or spectrum Click on the image and drag with the left mouse to outline a region on the image Maps will be acquired from the scanned region During TruMap acquisition a pro gressing green line is the map acquisition line followed by a yellow map processing line A layered image element maps and an electron image s SE BSE are displayed You can choose how you wish to view your data from Standard Interactive or Summary view available from the drop down list Adjust the slider bar to choose the number of maps per row The layered image allows you to see the X ray maps overlaid on the electron image You can add or remove an X ray map from the layered Image combined Electron and X ray map image by toggling the Layered Image icon in the top left hand corner of each map If you have lots of maps it may be useful to minimize some of them pressing the minimize icon 2 in the top right hand corner of each map You may want to delete a map from the analysis completely In which case press the delete icon Ei in the top right hand corner of each map This means this element will not be identified automatically AutoID and will be excluded from the current analysis Note If an element is present in a specimen deleting or excluding it will affect the TruMap results EDS SEM
73. has the same effect weakening the signal significantly or possibly remov ing the signal altogether If coating is necessary keep the coat thickness very thin typically 2 5 nm If the coating is too thin the conductive material will not be sufficient to dissipate the charge If the coating is too thick the signal to noise ratio will decrease significantly result ing with poor EBSPs SEM settings FSD imaging generally requires relatively high probe currents and accelerating voltages The backscatter diodes are less sensitive at lower accelerating voltages lt 5kV and work best in the range 15 30kV The FSD image signal increases significantly when the probe current is increased and ideally must be above 2 5nA You might need to increase the probe current for forescatter imaging and then decrease the probe current for EBSD analyses In variable pressure low vacuum mode FSD imaging is possible at low chamber pressures e g below 40 Pa 0 3 Torr Sample detector geometry One of the most important factors for getting high quality forescatter images is the sample to detector geometry The ideal geometry allows all silicon diode detectors to collect elec trons that have been reflected off the surface of the sample To achieve the best FSD image you need to vary the focal working distance and the detector position If the geometry is incorrect the signal might be too weak for the diode detectors to be useful even if the sample
74. in interpreting the final result since if for example the element list is incomplete there will be serious errors in the result even though the total is 100 This is often used as an expedient where the beam current is unstable or the specimen is unpolished With normalization you need not worry about beam current fluctuations but you must take care not to omit any major elements from the element list because this will not be obvious in an analysis total which is forced to be 100 Element List You can select a different type of element list depending on how you want your spec tra spectrum to be quantified e Current Spectrum 188 4760 FD or INSTRUMENTS The Business of Science If this option is selected each spectrum will be quantified using the elements confirmed in the Confirm Elements step for the current spectrum e Fixed List Select this option if you wish to define a list of elements with which to quantify your spectra For example you may only wish to quantify your spectra using certain elements if you are con stantly quantifying similar spectra Define your Fixed List using the Periodic Table To include an element in the list click on the element symbol on the Periodic Table and press Include or double click on the element symbol e Fixed List and Current Spectrum Select this option when you know what elements there are in your specimen and you also wish to include any other element that may
75. is displayed as Drift Proximity The proximity display shows a colored bar that extends from green to yellow to red as the limits of AutoLock are reached The bar will be full and in the red if AutoLock is exceeded i e the scan region has drifted to the edge of the image Selected Item Details of the drift correction for an item selected on the Data Tree in the current Project are displayed here See Also AutoLock Settings below FAQs about AutoLock on page 140 AutoLock Settings AutoLock is set to Off Auto or Custom mode In the Auto mode the system chooses a set of default settings In the Custom mode you can specify the AutoLock settings shown in the screen shot below ch Auto Lod cS ettings AutoLock Settings Off Auto Custom Tracking Image image scan sme im Dwell Time ius 10 Frame Time secs 05 Input Signal SE Scan Settings Use Automatic Measurement Interval Putok Aloe In field Extended nek Maimun Catt Sof eld Width 50 2x zoom Fi Use Predictive Comection Reference Interval secs 10 Tracking Image 138 EDS SEM Oy 45O ND INSTRUMENTS The Business of Science You need to specify the tracking image settings to use including the resolution Image Scan Size speed Dwell time in us and Input Signal Image Scan Size You can choose the size of the reference tracking image from the Image Scan Size drop down list The availabl
76. is labeled as Line where is an auto increasing number under the current site Site 1 as shown below Project 1 a Specimen 1 4 lt gt Sitel Electron Image 1 Line Data 1 Line Data 2 Line Data 3 Line Sum Spectrum Mg Kal 2 Ti Kal Cr Kal Mn Kal Fe Kal Br Lol 2 The Line item is the container for EDS Data All linescans and the sum spectrum are contained within the EDS Data The Linescans can be processed as Windows Integral Linescans TruLines or QuantLines The Data Tree is populated with the appropriate Linescans on selection of the processing option Windows Integral Lines The standard element linescans obtained from can the counts in the element energy windows including the background TruLine The Linescans are corrected for peak overlaps and any false variations due to X ray background QuantLine The linescans are processed to show relative per centages of each element by weight or number of atoms The label of the element linescan is composed of the element symbol followed by the lines series used for TruLine Window Integral data analysis For example Cr Kal is the label for a Chromium Linescan obtained from the Kal line Line Sum Spectrum The sum spectrum is called Line Sum Spectrum ive The region the spectrum comes from is visible on the electron image This is the same region as where the linescan data is acquired from 90 gt 420 PD EDS SEM INSTRUMENTS The Bus
77. make a change to the Quant Settings and press saved to be used when you do quantification next time the new settings are 190 EDS SEM Oy 45O ND INSTRUMENTS The Business of Science Element Lists Any list of elements in the software can be split into the following three categories Pre defined Elements elements expected in specimen Identified Elements typically based on automatic peak identification Auto ID Fixed List used for Quantitative analysis Pre defined Elements You may have prior knowledge of your Specimen and know what elements to look for Examples I want to look for a particular list of elements I am not interested in any other ele ments 1 may want to see their labels on spectra their X ray maps or both I want to see these even if the element is not present I know what s in my sample I want to look for a specific set of elements I want to see these even if the element is not present but I would like to know if there is anything else in my sample too You can define these elements in the Pre defined Elements tab in the Describe Specimen step If you want to save the Pre defined Elements to a profile you must first press Save to Profile button then save the profile via the drop down menu When you want to analyze your Specimen you can load this profile or another profile by pressing the Load Profile but ton in the Describe Specimen step as sh
78. map data from a region 1 In the toolbar on the left of the layered image click an icon then outline the region 451 Outlines a rectangular or square feature or area on the image Outlines an irregular shaped feature on the image Outlines an oval or elliptical feature on the image 2 Click and drag the mouse on the image to outline the region 3 Release the mouse button Map data will be acquired according to the current resolution If you wish to use a different step size to the one determined by the resolution type in the required step size Map Display If you have chosen to view the maps in addition to your acquisition area you can see the lay ered image maps both EBSD and EDS if selected and electron images You can also choose how to view your data from Standard Interactive or Summary view from the drop down list above the maps Map data will be acquired according to the resolution currently set under Settings If you wish to use a different step size to the one determined by the imaging resolution type in the required step size Layered Images Layered images are composite images that show you the X ray or EBSD maps overlaid on the electron image If you chose to acquire both EDS data and EBSD data two layered images are automatically created EDS layered image consists of an electron image and X ray maps whose selection is defined according to the current settings EBSD layered image
79. mass thickness is defined as the product of density of the material and its thickness Hence to determine the thickness the density of a layer must be known and be entered into the model Therefore it is important to realise that the value of the density directly affects the measured thickness Defining the thickness of each layer Enter the thickness of each layer in nm Simulated Spectrum conditions Specimen tilt Elevation and Azimuth Select a spectrum from the data tree which acts as the template spectrum Values for the tilt elevation and azimuth angles are read directly from this spectrum In addition the beam calibration is also read The values for the tilt elevation and azimuth angles displayed are of the template spec trum and are not editable 297 298 Livetime s The Livetime is user selectable When you select a spectrum in the data tree the Livetime for the simulated spectrum is set to match to that of the selected Spectrum Beam current factor The beam current used for simulation is equal to the beam current factor times the beam current used for beam measurement when cal ibrating This is user selectable When you select a spectrum from the data tree the beam current factor is reset to one One is the value if the beam current is the same as that used for the beam calibration for the template spectrum Calculated Count Rate kcps This is the number of counts in the simulated spec trum divided by t
80. may not need to optimize for many months How to perform Energy Calibration Energy Calibration requires the acquisition of a high quality spectrum from a suitable element from which details of the spectrometer gain are calculated and stored You can use an element as an energy calibration standard as long as the calibration peak is not overlapped by other peaks There should not be any peaks within 100 eV of the cal ibration peak To perform Energy Calibration follow the steps Select Energy Calibration from the Calibration Routine drop down list Select an element from the Calibration Element drop down list Get the element standard in the field of view of the microscope Adjust the working distance to the recommended value and the beam current to achieve an optimum count rate gt START Press to start acquisition of the calibration spectrum The current set tings will be used to acquire the spectrum A window will be painted across the peaks of the element X ray line series A progress bar near the top of the Calibrate window displays the estimated time for the completion of calibration spectrum acquisition On completion of spectrum acquisition a message is displayed asking you if you wish to perform the Energy Calibration Press Yes if you wish to perform the Energy Calibration Note that the details of the Energy Calibration can be found in the Spectrum Details dialog in the Calculate Composition step
81. more detail using any of the Available Templates To view result select the template that you wish to use Available Templates Quant Result Details Summary Table Single Spectrur Label Comparson of Results Two Spectra Element List Type summary Table Multiple Spectra Processing Option Full Results Table customizable Single Spectrum Ratio Standard Element a p E e p a E Ra ad l spectrum Details Details Ratio Standard Line Diagnostics Table customizable Single Spectrun Specimen Density T TT m an ore 1 _ Ur Cec Ss Le J spectrum Processing Processing specimen Thickness Automatic Line Selection Thresholding Deconvolution Elements Copy Spectrum 2 Current Spectrum f All Elements Silicon K seres 0 nm 0 g cm Enabled Disabled None Ifyou want to see a comprehensive set of results from a single spectrum then choose the Full Results Table customizable Single Soectrum template and which ever spectrum is highlighted in the Data Tree will have its results shown in this tem plate To populate a multiple spectra template hold the Ctrl key down while choosing spectra on the Data Tree and then press the Add Selected Spectra button at the bottom of the Data Tree window 359 Data View Current Site Data Tree Mineral Sample d Map Data 1 VG Spectrum 2 Fo C Spectrum 4 Do Cp o TE Spectrum 7 d Line Data 1 gt Site3 Add Selected Spectr
82. of X rays changes dramatically at the carbon absorption edge energy Any other materials in the detector window will cause a sim ilar absorption artifact The artifact at carbon will give a significant carbon peak area For example if the thickness of a carbon film on silicon were being determined the artefact could make the film thickness appear larger than it really is The Correct for window artefacts feature takes account of all absorption steps due to whatever window material has been used in the detector and removes the systematic errors caused by such artefacts The effect of the correction can be seen by performing analysis with and without the box checked Quant Standardizations Select whether you wish to use the Quant Standardizations as supplied by the factory note that the extended set is also available or the User defined set of standardizations If you need accurate results although good results can be obtained by using factory stand ards you can improve the accuracy of your quantitative results by using your own standards Standardize In AZtec quantitative analysis can be carried out without the need to measure standard materials since your AZtec system is supplied with sets of factory standardizations If the factory standards are not good enough then you must make standards As a rule of thumb we recommend that you analyze a well characterized material which is typical of the sample you will be working on No
83. of individual spectra by selecting the color from the drop down list in the compare table To change the line thickness of individual spectra select it from the Line Thickness drop down list in the Compare table To apply the chosen line thickness globally select it from the Compare Spectra Settings from near the top of the Compare viewer Normalize 120 EDS SEM OXFORD INSTRUMENTS The Business of Science Normalize is a useful function for comparing spectra acquired using different input X ray count rates such as spectra acquired with two different beam currents Note that you can normalize spectra using a point or a region Normalize Spectra Point e Select this option from the toolbar near the top left of the Compare Spectra screen e Double click in the spectrum to set a normalization point along the X axis e A window is drawn on either side of this point The spectra in the Compare viewer are scaled to the average value of cps eV Y axis in the window Normalize Spectra Region e Select this option from the toolbar near the top left of the Compare Spectra screen e Click and drag to set a normalization region along the X axis e The spectra in the Compare viewer are scaled to the average value of cps eV Y axis in the normalization region selected in the previous step Smooth The Smooth function is available from the context menus of the spectrum viewer This is use ful when comparing spectra where s
84. of the image is Zoomed and rotated above the Linescan viewer This action aligns the defined line horizontally to match the x axis of the Linescan viewer Element linescans start to populate in the Linescan viewer from in the top right quad rant as the data is being acquired as shown in the next screen shot 20 gt STOP Settings Display Stacked Settings Electron Image 1 All Elements 16000 Pai Ti kal Cr Kal 12000 uh tt te nee Mn Kal Line Data 6 n ca ll a Fe Kol T i g000 a Mg Kal_ O Kal 4000 a A Kal an cial ah Wa 200 400 600 800 Minimised Lines Mode Selected Element Details In the bottom right quadrant you can define energy windows and configure X ray line series from Selected Element Details AutoID can be used for initial display You can add or remove elements as you wish using the periodic table Linescan Details seyd uawa papajas Clear All Spectrum Viewer 260 EDS SEM OXF INSTRUMENTS The Business of Science The spectrum is available in the bottom left quadrant You can view the Line Sum Spectrum and navigate to the Confirm Elements step from within this component to manually confirm elements Confirm Elements ns Line Sum Spectrum 4 La a I li e Y oll CL Ll Dose atounadaonaatlererloenadaang 0 2 4 6 keV 261 Optimize nnna There are two components in the Optimize navigator Calibra
85. on the TEM system You can enter the values for Delay in seconds and Threshold in MeV per sec ond Mega electron volts per second When the X ray flux exceeds the threshold value for longer than the specified delay time the detector will auto retract The user will need to move the detector back into the chamber by pressing the In button If the overload condition persists the detector will auto retract again You can restore the default values for Threshold and Delay by pressing the Restore Defaults button if you have overwritten them e X act Detector The Detector Control has Thermal tab Thermal 486 Hardware Control Oy 45O ND INSTRUMENTS The Business af Science There are two buttons on the Thermal control tab Operate and Standby Pressing the Oper ate button initiates the cooling process and pressing the Standby button puts the detector in the standby mode EDS Detector Control Extended Mode Disabled Vacuum Status Under Vacuum Operating Status Cold Standby The Thermal control tab displays the current operating status of the detector State Description Standby Cooling is powered down Allows power save and detector longevity Steady orange LED Warm Detector is not ready for data acquisition Steady orange LED Cool Detector is ready for data acquisition Steady blue LED Warming Detector is warming after selecting the Standby mode Cooling Detector is not ready for data
86. or Element from Standard Compound standard as appropriate from the Perform Standardization section X ray line markers will be dis played for the selected element K lines are in red Llines in green M lines in purple and N lines in cyan Select the line you wish to standardize on from the X ray Line Series drop down list Standardize Having selected the element and the line for standardization press to perform the standardization The current and new values of standardization will be displayed Press to update the standardization The existing values will be over written by the new values You will be asked if you wish to use the new stand ardization for Quantitative analysis Oy E RD EDS SEM INSTRUMENTS The Business of Science Note The Accept button will be grayed out if the Standardizations file is selected for quant You need to deselect it in the Quant Settings dialog available from the Calculate Com position screen if you wish to standardize on any entry in this file In Calculate Composition step when you press Requantify the new standardization will be used and displayed in Quant Results Details if you select the Full Results tem plate Ifyou have not accepted the new values for standardization no changes will be made to the existing standardization Managing Standardizations Your system is supplied with a Factory Standardizations database When you use your system for the first time
87. or automatic gamma to maps dur ing acquisition depending on your pre selection of Auto Brightness or Auto Gamma See also Acquire Map Data Settings on page 211 Context Menu Map Viewer on page 223 How binning affects the quality of your data on page 373 Layer modes in the interactive map display on page 216 369 Construct Maps Construct Maps In this step you can select which elements to map and which ones to exclude You can change the default X ray line used for Window Integral Maps for any given element It is also possible to define energy windows whose widths you can specify yourself rather than using the auto width calculation Tools are provided to interrogate the map data to confirm the elemental composition of user specified areas of interest You can navigate to the Confirm Elements step from within the Construct Maps step To reduce the effects of noise in the maps you can apply a binning factor Map Details Map Details dialog allows you to choose elements you wish to include or exclude for map ping You may have pre defined the known elements in your specimen in the Describe Spec imen step You can map these elements by pressing the Pre defined button in the Map Details dialog There may be unexpected peaks in the spectrum You can use AutoID for selecting elements for mapping You can access Map Details option from s located at the bottom of the workspace Y Map Details ik speag awa papaes
88. position 489 Activity State Not Moving Moving In Moving Out Homing Auto Retracting Position The detector is not mov Ing The detector is moving into the chamber The detector is moving out of the chamber During calibration of the hardware the detector goes through a homing routine which ensures that it finds the correct zero position for the counter mechanism The Touch Sensor has been triggered and the detector has auto matically started moving out of the chamber The insertion distance from fully retracted position is shown in mm and can also be shown in the status bar This is important because it always shows the position of the detector and constantly updates when the detector is moving Touch Sensor Not Touching 490 The front part of the detector has Touch Sen sors and none of these sensors are currently trig gered One of the Touch Sen sors on the front of the detector is triggered Hardware Control The Business of Science Interlock State Some systems have an interlock between the scanning electron microscope SEM and the EBSD electronics The option is not available for all SEMs and the function also varies between systems On some SEMs the interlock does not limit the detector movement On other SEMs the interlock does not allow the detector to be inserted into the chamber which means that the detector cannot move in and if it is alread
89. present or not the The Business of Science Context Menu Item smooth func tion sub stantially reduces the Statistical fluctuation so that any real peak becomes more visible Include in Scaling Noise Peak Exclude from Scal Ing Shows the noise peak and includes its value when the context menu option Reset Scales is used Shows the noise peak but excludes its value when the context menu option Reset Scales is used Hides the noise peak EDS TEM 329 Confirm Elements ot Coni Elements This step has been designed to help you confirm the elements that have been identified by AutolD in your spectrum These elements are then used to create a confirmed elements list for qualitative and quantitative analyses Extensive tools including Element Series Markers Overlays Element Profiles and Show Candidate Elements are available here to assist you in confirming elements manually How to confirm elements Start with the largest peaks Press the question mark icon to select the Show Can didate Elements tool from the tool bar on the left hand side of the interface then double click on a peak in the spectrum viewer The candidate elements are dis played in a stacked spectra view on the right hand side of the window you can dou ble click on any of these elements to add or remove it from the confirm elements list Lead Pb Lal Double click to add or remove element
90. press on each element in the periodic table that you wish to select and then press the Include Exclude or Clear but ton AutoID Settings You can enable or disable AutoID during acquisition by checking or un checking the Perform AutoID during acquisition checkbox AutoID Confidence Factor The default value for the Confidence Factor is set at 3 You can use the slider to set the value The Confidence Factor is used to determine how AutoID behaves with regard to the sources of error Map Element Details The Map Element Details dialog allows you to configure the element maps The default X ray lines are used for element mapping unless you specify them You can select the X ray line for each element that you wish to map from the Map Element Details in the Element Settings tab or in the Construct Maps step You can define the energy window width for each element rather than using the default value You can select which elements to map and which ones to exclude See Also Auto ID Confidence Factor below Auto ID Confidence Factor If the Confidence Factor is set to a high value AutoID will find the most significant peaks but may miss small peaks that are close to the noise level If the Confidence Factor is set to a low value AutoID will detect small peaks but may pick up false positive identifications that are due to statistics or systematic errors By default we set the Confidence Factor to 3 which corresponds to the 3 si
91. quantification of light elements since the lower penetration at low kV will reduce the absorption correction m Analysis of a small particle inclusion or a film less than 10 um in depth since a smaller excitation volume will enhance the contribution from these features Reducing the kV may reduce the options for easy element identification A higher kV will excite the higher energy lines The Br K line will be excited by 20kV but at 10kV only the Br L line will be excited which overlaps with the Al K line Magnification 496 Hardware Control OXF INSTRUMENTS The Business of Science What is it The magnification of an image is formally defined as the ratio of the length of one line of the electron beam on the monitor to the width of the area scanned on the specimen However since monitors vary in size and the image may be printed magnification on its own is not enough to work out the size of a feature Why is it important Magnification is used by the software when calculating the length of the scale marker bar to display beneath all electron and X ray images The marker bar will scale with the size of the image and is a more reliable indication of feature size Which Magnification should I use Electron Imaging In order to see greater detail in your electron image increase the magnification of the micro scope This effectively means that the electron beam rasters over a smaller area of the spec imen Depe
92. registration This feature is available only if the mail server has been configured correctly Tip Alternatively you can register the license code with a new user name and password To set up the mail server 1 On the licensing server open the License Manager For details see section 1 4 2 Select the Settings tab 3 Enter the fully qualified domain name of the mail server for example mail e xample com 4 Click Save To request the new password 1 On the registration page click the Forgotten password link 2 Follow the instructions on screen 267 How do I upgrade my license If you are upgrading your license you need to deactivate and reactivate the license to pick up the new modules For details see the sections in the Software Licensing User Guide You will need to know the user name and password that was set at the time of registration If you forget the password you can recover it by an email method You need to know the email address that was registered with the user name If you do not know the user name and password you can activate the software product by registering with a new user name and password You will need the license code Note You can access the License Manager from Tools in Oxford Instruments NanoAnalysis group of programs 58 Getting started OXF INSTRUMENTS The Business of Science Moving data to another PC When you start a new Project a Project fold
93. resolution Process time 6 is the longest and gives the highest resolution but at some cost to maximum acquisition rate The longer the Process time the slower data can be acquired i e the higher the system Deadtime will be for a given input count rate The input rate is not affected by the pulse processor Which Process Time should I use When you start your application first time the Process Time is set to Default This is a suitable choice for many routine applications where you are looking for good resolution of peaks and fast acquisition For the first look at a specimen you should use a long process time 5 or 6 to start with in order that you do not miss any detail in your spectrum For example when identifying peaks particularly those closely spaced and overlapping it is important to get good peak sep aration Good resolution is also important for looking at a series of lines that are very closely spaced like an Lseries and process times 4 to 6 should be chosen Common overlaps include the Mo Land the SK lines If there are no closely spaced peaks then you can afford to use a shorter Process Time such as 1 3 which will enable you to increase the acquisition rate by increasing the beam current A compromise between acquisition speed and resolution should be found if there are peak overlaps When acquiring SmartMap data you should choose your Process Time carefully 1 You may have been working on a Specimen in either Analyze
94. single point on the linescan See Also Data Tree on page 85 249 Exporting the linescan data Right click on the linescan viewer to access the Export menu It has several different ways of exporting the linescans Save As Copy Print and Email The exported image includes the rel evant information from the Caliper or Show data values tool To export some or all of the data to a spreadsheet program such as Microsoft Excel i 2 e 4 See Also On the toolbar above the linescan viewer select Table from the drop down list To select all the data click one row in the table then press Control and A To select only some of the data click a row then drag or use click and Shift click Right click and select Copy Paste the data into your spreadsheet Toolbars on page 253 250 EDS SEM The Business af Science Extracting a single spectrum from the linescan You can examine the spectrum and element quantities at any point along the line 1 In the toolbar on the left of the image viewer click the Reconstruct Line Point Spec trum tool 2 Move the cursor to any point on a line in the linescan viewer 3 Click to extract the spectrum for the point into the project You can view the spectrum in the Mini View The data is also saved in the Data Tree with this icon sdo ls Extracting multiple spectra from the linescan You can examine the spectrum and element quantities at man
95. solution as an overlay on the EBSP Display Band Detection Shows the band detection area as a Area circle Display Bands Shows the Kikuchi bands Display Pattern Center Shows the pattern center as a green cross EBSD Pole Figure Viewer 215 You can control the default display of pole figures and inverse pole figures To temporarily change the current display right click it and use the context menu Projection Type Overlay Inverse Pole Figure on Sphere Show Great Circles Use 4 Digit Indices Offers a choice of the type of projection equal area or ster eographic Shows the location of the inverse pole figure within the sphere Shows the latitude and longitude lines on the sphere Selects the 4 digit index nota tion Generally the 3 digit index notation is used EDS Layered Image Settings You can control the default display of the layered image to include new X ray map layers EDS Linescan Viewer You can select the default line thickness in pixels for the linescans Default Line Thickness Offers a thickness from Thin 0 5 pixels to Thicker 4 0 pixels The default line thickness is Thick Description For any other thickness select User defined and move the slider bar Spectrum Viewer You can control the default display of the Soectrum Viewer To temporarily change the cur rent display right click it and use the context menu 16 Getting started Description V
96. that location and displays the value for each element in that location For example If no sigma threshold is applied to TruLine processing some values might be negative To see the sigma threshold setting go to the Tools menu select User Profile and then the EDS Ele ment Settings tab 396 EDS TEM Oy 45O ND INSTRUMENTS The Business af Science Comparing element quantities The Normalize Y Axis option is available on the context menu of the Linescan viewer when in Stacked view It allows you to compare linescans with very different maximum count rates and is useful in QuantLine displays The maxima of linescans are scaled to the full height of the viewer It allows you to view the details of the minima of linescans with low count rate Note that there is no Y axis on the normalized linescans because the absolute scale is mean ingless 397 Smoothing the linescans The Smoothing Factor option is available from the Linescan viewer settings It allows you to smooth the linescans after normalization for visual clarity as demonstrated in the screen shots All Elements Ti kal Cr Kal 18000 a Fe Kool 16000 Al Kol 14000 Br Leal 7 N Kal 13000 E 0 Kor i mal liu WWT F Kol 2 10000 ai i A HN ancl I 8000 6000 4000 2000 Typical linescan The Smoothing Factor uses moving averages to remove fluctuations of data The options available are 1 Nosm
97. the Optimize navigator Repeat the Beam Measurement as often as is required in order to check beam current drift For details of the Beam Measurement routine refer to the Calibrate help topic link below Acquire a spectrum from the specimen The spectrum will then be added to the data tree in the current project View the MiniQuant results on completion of spectrum acquisition Notes The Beam current must be the same for both the standard and specimen It is vital that the beam current is stable to achieve good quantitative analysis For accurate identification of peaks you will need to perform an Energy Calibration However the AZtec system has very stable electronics and therefore you may only need to calibrate the system once in several months provided the environmental temperature of the laboratory is fairly stable The Sensitivity analysis display in the Confirm Analysis step shows the effects of beam current variation In some analyses a 1 variation in beam current could give significant errors in results and therefore stability in beam current is important Display options You can display the components that you are working on such as image and spectrum using the controls on this toolbar located in the top right side of the screen You 284 LayerProbe OXF INSTRUMENTS The Business af Science have choice of displaying image and spectrum as shown in the screen shot below or just an image or
98. the Start and Stop buttons Choice of Weight and Atomic in the MiniQuant Map consistency Users can now save not only map colour selections directly to pro files from mapping navigator but also the AutoLayer assignment so that the same colours are used when going from area to area See Acquiring linescans on page 391 Construct Linescans on page 403 Acquire Map Data on page 363 and Construct Maps on page 370 Vil What s New in Aztec 2 0 SP1 SP1 contains mostly bug fixes localization help updates some usability modifications and one new functionality implementation New functionality Users will now have the ability to hide the noise peak in their spectra via the right mouse but ton this is a universal setting that once turned on applies to all spectra Oo gt Reset scales Export Peak Labels Annotations X Axis Y Axis Normalize Ca Fe Smooth Eoo n EATE AEEA RA RAA es ee A A O A Exclude from Scaling 0 5 1 1 5 2 Details Ta e O T ee VARANE i 15 i g AFUE JZTNTR LUTAN SESA ERE MEA y 0 0 5 ASSET EN 7A L5 2 A selection of bugs that have been fixed in SP1 m AZtec 2 0 stops working with LN2 detectors systems Irregular spectrum and mapping acquisitions were occasionally failing when a user draws a free hand acquisition area for spectrum acquisition of mapping acquisition would occasionally fail to start User defined energy windows in EDS mapping were not
99. the center of the field of view The acquisition area from which the data is collected is then a smaller area within the field but not nec essarily within the tracking image See the figure below In this mode the analysis will stop if either the acquisition area or the tracking image reaches the limit of the original field of view Acquisition In field no zoom area CENY ONS ON NSSE N Proximity 90 Y Tracking image i Full acquisition area What is Extended Field Mode mee EDS SEM Oy 45O ND INSTRUMENTS The Business af Science This mode requires that the image is zoomed at 2x 4x or 8x This reduces the size of the field being analyzed the acquisition area has to be within the tracking image area If the image is zoomed 2x then the center 50 of the image is taken for the tracking image If 4x zoom is used the inner 25 of the original image is used for data collection The amount of potential correction available is therefore larger when higher zooms are used 4x zoom extended field Prowmity 25 Trackibg image Full acquisition area Acquisitian area But What If I want to Maintain Subject Size When using extended field mode you can maintain the size of a feature on the image by ena bling Maintain Subject Size The magnification on the SEM is changed to maintain the same field of view based on the zoom that is selected Note This opt
100. the electron beam Carbon is generally the preferred coating material for microanalysis applications because of its minimal effect on the X ray intensities Gold is also commonly used for coating specimens since it increases the secondary electron yield providing improved SEM image quality However the number of peaks produced by the gold coating can cause overlap problems with the peaks of interest A guide for the desirable thickness range of coatings is of the order of 5 30 nm To minimize the effect of your coatings aim to make them as thin as is practically pos sible Thick coatings will for some samples result in poor analysis Effect of the Coating on the X ray spectrum The coating will have three main effects 1 Energy loss of the primary electron beam as it passes through the coating 2 Attenuation of the emerging X rays 3 The contribution of characteristic peaks to the X ray spectrum Thus carbon coated samples will always display a carbon peak in the spectrum In the software you can specify a coating element for a particular sample During spectrum proc essing any X ray peaks arising from this element are automatically deconvolved in addition to two other corrections loss of X ray intensity due to absorption of the emergent X rays reduction of primary keV Application of these corrections is particularly important for low kV spectra in particular 5 keV The final quantitative results could have sign
101. the maps and select the best ones to provide an effective color image that delin eates regions of different composition Maps will be auto brightness corrected and those that show similar structure will be assigned the same color Maps that are very noisy will be shown in grey The most significant map for each assigned color will be added to the Layered Image See AutoLayer on page 222 for detailed infor mation If your data contains a lot of noise binning might help you to achieve a better Auto Layer result Select the binning factor from the drop down list below the maps Data from Map Acquisition The Data Tree gets populated with the new items as data is being acquired as shown in the screen shot below 365 Electron image Data View leone It can be a secondary electron image at ee SE backscatter electron image BSE z Em or a forward scattered electron image a a Specimen 1 _ Appropriate detector hardware needs rA Site 1 9 be etane L eu can also import an image into the Project _ Electron Image 1 S Map Data Map Data 1 M EDS Data The EDS and EBSD Map data are con a Spect tained in the Map Data folder The EDS R ae Data folder contains Map Sum Spec Mg Kal Z trum and X ray Element Maps Ti Kol Cr Kal Mn Kal X ray Element Maps Two modes of mapping are available Window Integral Maps and TruMaps EDS Layered Image 1 To select the mapping mode press the Map Data 7 Map or TruMap butt
102. the number of maps per row in the Standard and Interactive displays Offers a choice of map display Standard you can add individual images or remove them from the combined image Interactive similar to Standard Links the zoom and pan of all the maps Summary a compact display where you can change the color of each phase Links images for manipulation of all layers using the Pan or Zoom controls Changes the brightness and contrast of the cur rently selected image or map Adds the selected phase map or electron image to the combined phase image Minimizes a map The Minimize icon is in the top right hand corner of each map This is useful if you have too many maps in view The map moves to the Minimized Phases tab below the displayed maps Removes a map or electron image from the phase analysis This icon is in the top right hand corner of the image 383 Settings Description Restores a minimized map to its normal size The minimized maps are on the tab below the dis played maps This icon is in the top right hand corner of each map Sets the color of the phase The list is available only in the Interactive and Summary map display See Also Analyze Phases on page 375 Processing toolbar These controls are at the top of the window above the phase maps Starts processing the element maps to create each phase map A Cancel button and a progress bar appear during the
103. use a long process time 5 or 6 to start with in order that you do not miss any detail in your spectrum For example when identifying peaks particularly those closely spaced and overlapping it is important to get good peak sep aration Good resolution is also important for looking at a series of lines that are very closely spaced like an Lseries and process times 4 to 6 should be chosen Common overlaps include the Mo Land the S K lines If there are no closely spaced peaks then you can afford to use a shorter Process Time such as 1 3 which will enable you to increase the acquisition rate by increasing the beam current A compromise between acquisition speed and resolution should be found if there are peak overlaps When acquiring SmartMap data you should choose your Process Time carefully 1 You may have been working on a Specimen in either Analyzer or Point amp ID where you have setup your acquisition parameters to optimize your quantitative analysis If you now wish to acquire SmartMap data and you think you may wish to recon struct spectra from your SmartMap data and then quantify these spectra you should maintain these acquisition parameters This means that you may have to acquire data with a long Process Time to maximize resolution but limit the maximum acquisition rate 2 You may have been working in either Analyzer or Point amp ID and you want to view the distribution of elements whose main peaks do not overlap as a map or a l
104. used for calculating the composition in the Quant Results Details list box Parameter Description Label Spectrum Label E g Soectrum 1 Element List Type Current Spectrum Fixed List or Combined List Processing Options All Elements Element by Difference Com bined Element or Oxygen by Stoichiometry Apply Coating Correction Enabled or Disabled 118 OXFORD INSTRUMENTS The Business of Science Parameter Coating Element Coating Thickness Coating Density Automatic Line Selection Normalization Thresholding Deconvolution Elements Factory Standards User Standards Pulse Pile Up Correction Detector File Efficiency EDS SEM Description E g Carbon E g 15 nm E g 2 25 g cm3 Enabled or Disabled Enabled or Disabled Enabled or Disabled None Selected Standardizations file supplied with the sys tem Standardizations file defined by the user Enabled Disabled Indicates file that has been used to char acterize detector Calculated File based Quant Results View The information displayed in the Quant Results View depends on which template has been selected You can view Spectrum Details Soectrum Processing and Diagnostics table in addi tion to quant results See Also Quant Settings on page 187 Element Lists on page 191 Compare Spectra amp MiniQuant Results on page 195 119 Compare Spectra Compare Spectra This step in both the Point amp ID and Analyzer Navi
105. user profile Click to start the image acquisition according to the cur rent acquisition parameters Click to stop image acquisition Acquisition stops at the end of the current frame Click again to stop imme diately If you navigate away from the step acquisition stops at the end of the current frame To change the acquisition parameters click the Settings cog on the Acquisition Toolbar to display a dialog You can select Image Scan Size Dwell Time us Input Signal the labels here reflect whatever was set during the installation for example SE BSE or FSD either Con tinuous Scan or Number of Frames and Frame Time secs If your specimen is drifting you can activate AutoLock to ensure that any analysis corresponds to the true loca tion on your image 347 Control Description Mixing Mode Combines signals from the diodes to form a mixed image Some options are available only if the required drop down list l l l diodes are installed and configured FSD only FSD Z Contrast uses upper and side FSD detector channel images Select this mode if you are inter ested in seeing density atomic Z contrast signal FSD Topo Orientation uses lower FSD detector chan nel images Select this mode if you are interested in seeing orientation contrast signal Custom include and exclude FSD detector channel images of your choice When you select either of the first two modes the soft ware automatically us
106. where you release the mouse Both spectra are scaled along the Y axis to the average value usually cps eV in the window Annotations Five tools available to add annotations on the current spectrum and the image are Caliper Angle Text Rectangle and Ellipse Select the tool by clicking on it and then click on the spec trum image to add annotation For example to add text select the Text annotation tool click 317 on the spectrum where you wish to enter the text and then start typing the text To delete annotation double click on it to select it and then press the Delete key on the keyboard Show Data Values With this tool you can view the Energy keV and counts in any channel of the spectrum Simply select the Show Data Values tool from the toolbar and then hover on spectrum The values will be displayed as you move from channel to channel Acquisition and Settings Toolbar Near the top of the Acquire Spectra window there are buttons for starting and stopping acquisition as shown below Acquire Spectrum START E STOP Settings Press the Start button to acquire a spectrum There is a Settings cog in the toolbar For details of settings see Acquire Spectra Settings on page 313 Compare Spectra amp MiniQuant Results Real time Compare and instant MiniQuant options are available in the Acquire Spectra Con firm Elements and Calculate Composition Comparison of Results Two Spectra template steps User can see results
107. will be included in the analysis If you have already created a User Profile with the Pre defined Elements in the User Profile Load from Profile dialog press r Clear All Pressing will deselect the Pre defined Elements from the periodic table and they will not be included in the current analysis The peaks for the Pre defined Elements if included in the analysis are labeled in the Acquire Spectra step MiniQuant will display the quant results for these elements as Wt or a bar chart The Pre defined Elements will be marked as Pre defined in the Confirm Elements list box in the Confirm Elements Step There may be other elements in the Specimen which are identified by AutoID routine if the Perform AutoID during acquisition option has been checked in the User Profile dialog 344 CX KO IRD EDS TEM INSTRUMENTS The Business af Science Tip Right click on the Project or Specimen in the Data Tree and select Edit Notes to write or edit notes in any step of the Navigator See also Element Lists on page 191 Data Tree on page 85 Mini View on page 93 Step Notes on page 94 345 Scan Image Scan Image In the Scan Image step you can acquire an electron image into a Site A Site is like a folder which contains images and analyses for a particular area on a specimen For EDS if you do not want to collect an image and just want to acquire spectra you can skip this step and go stra
108. will be seen around 12 8 keV Notes The pileup correction algorithm assumes that the count rate at every energy is constant throughout the analysis period Therefore the correction works best when analysis is per formed on single pixels points or areas of same composition Bad results may be obtained if the beam is rastered over an area where composition is changing or if a spectrum is recon structed from a SmartMap over a region where the composition is changing 156 The Business of Science EDS SEM Context Menus Image Viewer A number of useful shortcut menus available as right mouse click in the image viewer are shown in the table below Context Menu Item Rescale Image Set Image Colors Export Annotations Show Acquisition Areas Fit Image to Display Fill Display with Image Color Bar Header Scale Bar Show Con trast Brightness Buttons Color Key Save As Original Res olution Save As Copy Print Email Settings Show Select All Style Delete Show All 157 Show Selected Show None Show Short Names Details Peak Labels Peaks in the spectrum are automatically labeled during acquisition if AutoID is enabled in Pre defined Elements tab in the Describe Specimen step You can configure peak labels from the Peak Labels tab available in two places in the soft ware a User Profile Confirm Elements step Default Peak Label Behavior
109. without having to move away from the acquisition mode Using these options you can See your results during analysis Compare your current spectrum to a control spectrum during acquisition a View MiniQuant results in a table or a bar chart Click B in the top right corner of the Spectrum Viewer in Acquire Spectra Confirm Ele ments or the Calculate Composition window to access the Compare amp MiniQuant options e In the above example Spectrum 1 is the current spectrum and Spectrum 2 is the comparison spectrum You can select the comparison spectrum from a Project currently available in the Data Tree It can be from any Project any Specimen and any Site of Interest currently available in the Data tree To choose the comparison spectrum click on the down arrow Spectrum 2 in the above example Spectra available in the current Project Specimen and Site of Interest are displayed as below 318 EDS TEM ON INSTRUMENTS The Business of Science Proect1 Speamenil Click on the spectrum in the display to select it for comparison The selected spectrum will be overlaid as a line spectrum over the current spectrum The MiniQuant results are displayed in a table as shown in the example below Spectrum 1 Spectrum 2 3 Wt c W o The results are displayed as wt weight 319 The statistical error is displayed as o weight sigma for the calculated wt It is the overall
110. you had many solutions gt 10 then this may take a long time Adding Phase for Acquisition The phase from the solution that you consider the correct solution can then be added to the usual list of phases for acquisition in Describe Specimen by pressing the Add Phase for Acquisition button You may wish to experiment solving with this full list of phases and a link to the Optimize Solver step is provided See Also Optimize Solver on page 444 AB s Hardware Control The Business of Science Hardware Control In this section various software tools that control the hardware are described Detector Control 6 88 ccc cece cece cece eee 484 EBSD Detector Control 6 489 Microscope Control _ 2 2 2 2 2 2c e eee cccc cece ee ee ec ceeeeeees 493 483 Detector Control There is a separate control for EDS and EBSD detector hardware which provides information about the hardware status Each control is accessible from the Detector Control icon in the right hand side of the Status bar The Detector Control is displayed as a pop out dialog The EDS Detector Control software is described under three current EDS detectors e X Max Detector In the case of X Max detectors there are three tabs Thermal Position and Protection EDS Detector Control Thermal Operating Status Cold Position ee Protection Thermal The Thermal tab displays the current operating status of the detector The pos
111. you press located on the right hand side of the Status Bar the Microscope Control is displayed as a pop up window The current value of each parameter is displayed in the appropriate entry box in the Micro scope Control as shown in the screen shot below In this example the Column tab is selected Microscope Control Column DefaultMPO Current Values New Values sigs Magnification 100 100 Working Distance mm 10 00 10 00 High Voltage kV 20 00 20 00 The exact way in which each of its functions operates depends on the facilities available on the microscope on which the EDS system is installed Where possible parameters can be changed either from the electron microscope controls or the Microscope Control and both systems will be updated accordingly In some cases it may be possible that the parameters from the microscope are read automatically but can not be changed in the Microscope Con trol If Microscope conditions can not be read automatically you will have to manually enter the values see below It is important that the correct values are entered such as WD working distance and magnification as these will be used during quantitative analysis and image cal ibration Column parameters such as working distance magnification and high voltage are also impor tant for the EBSD systems performance so if these are not read automatically then they must be entered manually How to change parameters in Microscope cont
112. 0 by default It should be noted that if a pure element is specified which is normally present in the gaseous state then the density is given a default value of 1 0 g cm3 Additional notes When adding a material if a material with the same name Is already stored in the database you will be warned and given the option to overwrite the existing entry If you wish to delete a material from the database select it and press delete Note that a warn ing will be shown before deletion 295 Simulate Spectra cece mE 1M oq Simulate Spectra In this step you can simulate a spectrum based on the model of a layered structure This may be helpful when setting up the experiments or when refining the model of a partially unknown specimen A spectrum is selected from the data tree which acts as the template spectrum for synthesizing a spectrum Parameters such as geometry settings and beam cal ibration will be read from this spectrum It is important to note that the template spectrum must be beam calibrated Spectrum acqui sition parameters are then selected in the various fields and a spectrum Is simulated To simulate a spectrum 1 Set up a model including all of the layers and the substrate of the specimen you want to simulate either using the Describe Model step or the interface provided in the Simulate Spectra step Save the model by pressing the Save button Your model will be saved in the User Profile 2 Select
113. 2 22 22 2 cece cee cee cece cece cece cece cece ceeceeeeeeeeeees 496 Index aa ess ees Sets eres eee E EERS 499 XXI Getting started The Business of Science Getting started The unique features of the user interface are described in the Application overview followed by the Guided tour of the Application The details about the software licensing are covered in the frequently asked questions Application overview 2 2 22222 c cece cece eee e ee eee ee eee 2 FAQs about Software Licensing 20222 2 222 eee eee eee 56 Moving data to another PC 2 2222 59 Application overview There is a great deal of flexibility in the user interface You can configure the workspace the way you wish to work and save a custom configuration layout to come back to every time The main application consists of the workspace in the middle area It is supported by a side panel on the right containing Project Data Mini View and Step Notes You can remove each of these components from the view if you wish Dockable and Floating Window Panes The window panes are docked as the default configuration of the user interface You can un dock and free float them Click and drag them wherever you want them in the interface or to a second monitor Re sizable Windows and Dialogs Windows and dialogs can be resized by clicking and dragging their edges The main appli cation window can also be re sized
114. 2000 12000 11000 e pan 1 LI ia i 10000 10000 aat a rnrn 9000 9000 afata a Phr LE i LI 1 ir LI U i ar aTa g Mii 7 i PULAJ wrt a i ul i i ar tes Beal af aTa g ee D L i mura 000 ar ha Cira Le a r Prats a th j AULA z E j J E la a 4 f 4 ov i H il i i F a aTi k an F E LA Pa A LI i hats a tr Lr Original data at 1 um spacing Binned data 374 EDS TEM Oy 45O ND INSTRUMENTS The Business of Science Analyze Phases cece l Analyze Phases In this step the software automatically converts X ray maps into phase maps The phase maps help you to see the constituent elements of the phase and how the phases are dis tributed over the specimen The window has several sections Element map Individual Combined phase phase maps map image gt pimag and the elec tron image Minimized phase maps Phase Details Spectrum The individual phase maps top right are presented according to the distribution and size of each phase The first maps show large areas of closely grouped ele ments Later maps show smaller areas that are more finely distributed You can change the colors in the phase maps to better represent interesting groups of ele ments or phases On the Image tab top left you can view any image in your project such as the EDS layered image The Phase
115. 5 is strongly not advised as it could mean over exposure e Noise Level This is a useful tool to monitor the noise level as you change parameters such as gain bin ning and exposure time The value is the percentage of noise in the image where 100 cor responds to no signal but all noise whereas 0 corresponds to all signal e Time per Frame The time per frame is the time taken for the camera to read out one EBSP Depending on the camera settings this time can differ slightly from the requested integration time Image Processing Settings Initially any small clusters of pixels arising due to defects or scratches on the phosphor will be masked out and disregarded in further processing of the EBSPs such as background cor rection Background correction methods as well as frame averaging are then available to use to improve the quality of the EBSPs The processed EBSP is displayed below the unprocessed EBSP to show this improvement Once the selection is made these settings will be used when ever an EBSP is acquired It should also be noted that automatic stretching of the processed image takes place in order to make full use of the dynamic range in the image Background method An EBSP consists of a series of relatively weak Kikuchi bands on a strong non linear back ground Removing this background produces a much clearer EBSP When a background cor rection method is applied the EBSP pattern is divided by a model of the background and the
116. A HN ancl I 8000 6000 4000 2000 Typical linescan The Smoothing Factor uses moving averages to remove fluctuations of data The options available are 1 Nosmoothing applied 3 Data averaged over three points 5 Data averaged over five points As an alternative way to reduce the effects of noise in the linescans you can apply a binning factor Binning is particularly effective when using TruLine See Also How binning affects the quality of your data on page 373 248 Mg Kal_2 ii PT ri Ct igi i ral a 180 210 240 2 0 300 a 30 Linn Smoot EDS SEM Oy 45O ND INSTRUMENTS The Business of Science Linescan Data The data tree contains a Line item under the Site this is the container for the line data By default this is labeled as Line Data where is an auto increasing number under the cur rent site Site 1 as shown below Project 1 ig Specimen 1 4 Sitel _ Electron Image 1 Line Data 1 Line Data 2 Line Data 3 y CA mora Line Sum Spectrum Mg Kal_ Ti K l Cr Kal Mn Kal Fe Kal Br Lol 2 The Line item is the container for EDS Data All linescans and the sum spectrum are contained within the EDS Data container For details right click the icon Taa The sum spectrum is called Line Sum Spectrum OS AN The name of the element linescan Line TruLine or QuantLine is composed of the element sym bol and the line A spectrum extracted from a
117. AZtec User Manual Issue 2 1 INSTRUMENTS Oxford Instruments 2013 The Business of Science Copyright The Business af Science Copyright Copyright 2010 2013 Oxford Instruments Nanotechnology Tools Limited trading as Oxford Instruments NanoAnalysis All rights reserved What s New in AZtec 2 1 AZtec 2 1 release contains the following new functionality ED LayerProbe m QuantLine AutoPhaseMap LayerProbe LayerProbe provides a non destructive tool to measure the thickness and composition of sur face and subsurface layers in thin film structures It integrates AZtec s robust quantitative analysis routines with a powerful thin film analysis engine for reliable results Performs non destructive analysis with minimal sample preparation Predicts solvability and optimum experimental parameters to enable reliable precise measurements Analyses layers down to 1nm thickness Handles total structure thickness up to several microns Includes a simulation tool to generate simulated X ray spectra of thin film struc tures Precise limits depend on the sample and can be determined using the Solvability Tool sup plied with the software See LayerProbe on page 270 QuantLine for SEM and TEM Quant LineScan determines elemental concentration variations across a user defined line on the sample Results can be viewed in either a Schematic linescans for each element or A table showing t
118. Compare Spectra 0 22 2 2 cece eee cece ee eee eee 120 275 Describe Specimen o Describe Specimen In this step there are two tabs Summary and Pre defined Elements Summary In the Summary view you can write notes on the Project and the Specimen present in the Project For convenience you can also copy images diagrams and text from other doc uments emails and paste into these windows Notes are saved with the Project and you are allowed to edit notes in any step of the Navigator It helps to capture the important infor mation during the analysis Click with the right mouse button on the Project or Specimen in the Data Tree and then select Edit Notes to write modify the relevant notes You can add new Specimens to the current Project by pressing the New Specimen button New Specimen Specimen 1 Click on the Specimen in the Project Overview dialog This action displays the Specimen Notes for Specimen 1 text box Here you are provided with the text formatting tools You are allowed to write notes about each Specimen and save them You can add coating information for each specimen This information is used for the cal culation of the quantitative results Specimen Coating Information EB The specimen has been coated with Carbon Thickness nimi Density q cm3 You have access to the periodic table for choosing the coating element for each Specimen Two parameters coating density and thickn
119. D displayed below the EBSP in the field mode The undistorted and distorted EBSP 9 Click Calculate This calculates values for the dipole field strength and an X offset A correction factor based on these values is then applied to all patterns if the option is selected The corrected image appears below the undistorted image and should closely resemble the undistorted image Note that the black parts in some of the corners of the EBSP are ignored by any pattern solving and will not affect your anal ysis The corrected EBSP 10 Click OK to return to the Optimize Pattern step where you have the option to apply the correction factor to all subsequent EBSPs Additional notes If this correction has been applied to your data you can see this by checking the details of the data 441 During the calculation if both EBSPs are identical for example the distorted EBSP has been snapped twice in error the software reports an error and a correct pair of EBSPs should be collected Optimize Pattern Toolbar 442 Moves the image Click the Pan tool then click and drag the image Use the mouse wheel to zoom in and out Adds annotations to the current image The tools include Caliper Angle Text Rectangle and Ellipse Click the tool then click on the image to add annotation For example to add text click the Text anno tation tool then click on the image where you want the text and Start typing
120. EBSPs where no solution was found m All Patterns without Solving Stores all the EBSPs s but they are not solved In addition you may select the type of Storage Format compressed or uncompressed Note that storing the EBSPs significantly increases the file size however it is necessary for later reanalysis of the Map Data Include EDS Check this option if you wish to acquire EDS data with your EBSD Data If selected the EDS mapping settings will appear Number of Channels Select number of channels from the drop down list of Auto 1024 2048 or 4096 4K with which you wish to display the spectrum The number of eV channel will depend on both the energy range and the number of channels you select Energy Number of eV channel Range keV Channels 458 EBSD OXF INSTRUMENTS The Business of Science In the Auto mode the software checks for the energy range selected and sets the appro priate number of channels Energy Range keV Select a spectrum energy range from the available options of Auto 0 10 0 20 or 0 40 keV from the Energy Range drop down list An appropriate energy range should be selected in conjunction with the current microscope accelerating voltage If the accelerating voltage is above 10 kV in order to view lines which may be excited above 10 keV the 20 keV range should be chosen Below 10 kV it may be more appropriate to choose the 10 keV range since no lines above 10 keV will be excited
121. ENTS The Business of Science Describe Specimen A Describe Specimen In this step there are two tabs Summary and Pre defined Elements Summary In the Summary view you can write notes on the Project and the Specimen present in the Project For convenience you can also copy images diagrams and text from other doc uments emails and paste into these windows Notes are saved with the Project and you are allowed to edit notes in any step of the Navigator It helps to capture the important infor mation during the analysis Click with the right mouse button on the Project or Specimen in the Data Tree and then select Edit Notes to write modify the relevant notes You can add new Specimens to the current Project by pressing the New Specimen button New Specimen Specimen 1 Click on the Specimen in the Project Overview dialog This action displays the Specimen Notes for Specimen 1 text box Here you are provided with the text formatting tools You are allowed to write notes about each Specimen and save them Pre defined Elements If you know what elements are present in your Specimen and you only want to see peak labels or X ray maps for those elements then you can select them in the Pre defined Ele ments tab Press the Pre defined Elements tab to access the periodic table If you wish to enable the AutoID option check the Perform AutoID During Acquisition option 2 3 Summary Specimen Geometry Pre
122. Fixed List are defined in the Quant Settings dialog which is available in the User Profile and the Calculate Composition window Note that the Fixed List is only used for calculating composition in quantitative analysis Example I want to do quantitative analysis on my glass samples and want to compare results from one batch to another batch I am always looking for the same specified list of ele ments You can specify the Element List for Quant from the three available options in the Quant Set tings dialog as shown in the screen shot below Element list Buren seer Select an Element list for the Fixed List quantitative analysis from Fixed List and Current Spectrum the three options Iron Element Quant Line Fixed Weight Iron uth ee Fe and Ti are selected as the Fixed List elements but you can overide the choice if required Add element n Remove element Clear all elements Element List Quant Element List Details Current Spectrum 164 EDS SEM OXF INSTRUMENTS The Business af Science This list includes the Pre defined Elements and elements identified by Auto ID and manually using the Candidate Element tool Fixed List You select the Fixed List option if you know what elements you wish to quantify Choose the elements from the drop down list as shown in the screen shot above Fixed List and Current Spectrum To quantify the elements in the above two lists sele
123. General Performance amp Other EBSD Improvements a Faster Reanalysis Improved speed of the phase search in Phase ID CTF Channel Text File export TIFF export of EBSPs with both CPR and CTF format EBSD Reporting templates for mapping and Phase ID EDS sum spectra can now be extracted from combined EDS EBSD maps Top Tips Movie A Top Tips movie will be installed on to the PC desktop when version 2 0 software is installed The directory C Users Public Documents Oxford Instruments Nano Analysis Documentation The movie reveals the lesser known but useful functionality in the software Training CD A Training CD is now shipped with every system The CD contains movies on the general oper ation of the software XV Contents The Business of Science Contents 0 Copyright cn i What s New in AZtec 2 1 0 000000000 0000000000000000 e eee eens ii What s New in Aztec 2 0 SP1 6 8 88 c nce eee oaoa anonn viii What s New in Version 2 0 2 000000000 0a cece ence eee eee cece ccececeeeeceeeees Ix COMIC GINES settee fhe esters anana eannan nese ebicunahe suenclsaiege bine gaccerm xvii Getting started 2 2202 ccc cece eee eee cece ee eee eee eeeee 1 Application Overview 2 222 222 2 eee ce ccc ce ec ccc cc cece cee ec cece ceeecceeeeececeeeeseeeeeess 2 VU ACO Seca stk ee eee eee neue EPa 5 MG NU Balt ccc 2acccsc denne dacacawenweodcanceronmneculiowmawsdeeacabenaenupceae canoes oee
124. ID Custom 2 222 022 2 cece cee cee eee eee eee ee 199 Acquire and Confirm 22 2222 cee eee ceeeeceeeeeee 201 Recommended way of working in Point amp ID Custom OGG goes poet ese E OE 202 Map Guided 2 0 2 2 occ ccc cece cece cece cece cceeeceeeceeeees 204 Acquire Map Data 0 0 22 cee cee cee eee eee eee eee 205 Construct Maps 0 22 cece cee eee ee ee eee 219 Analyze Phases 00 2 02 c eee cece ee eee ee eee ee ee eens 226 Map CUS COV assoc hse bene neeciceewnanneeasseweseebancetawneeeecad 236 Acquire and Construct 20 00 22 cece cece ee cece ec eeeee 237 Linescan Guided 22 2 0 22 cee cece ee cece ee eee eee 239 63 Acquiring NINES CANS cas ta yet te en uneudeslateedietees 241 Displaying and manipulating linescans 243 Measuring the distance between two points 245 Viewing element counts and percentages 246 Comparing element quantities 00 220 20002 247 Smoothing the linescans 0 2000 0 22 e eee eee eee eee 248 Linescan DACA sens ce cesioed derucdeumwaceuercear eases EEE 249 Exporting the linescan data 0 00 220 eee e ee eee 250 Extracting a single spectrum from the linescan 251 Extracting multiple spectra from the linescan 252 Construct LINCSCANS cc2 oauc ct Sosieivs se dehtidee lee siieeeds 255 Linescan Custom 22 c2025
125. If you have already created a User Profile with the Pre defined Elements in the User Profile fs Load from Profile dialog press P Clear All Pressing will deselect the Pre defined Elements from the periodic table and they will not be included in the current analysis The peaks for the Pre defined Elements if included in the analysis are labeled in the Acquire Spectra step MiniQuant will display the quant results for these elements as Wt or a bar chart 7 The Pre defined Elements will be marked as Pre defined in the Confirm Elements list box in the Confirm Elements Step There may be other elements in the Specimen which are identified by AutoID routine if the Perform AutoID during acquisition option has been checked in the User Profile dialog Tip Right click on the Project or Specimen in the Data Tree and select Edit Notes to write or edit notes in any step of the Navigator See also Why are specimen coated on the facing page Coating Techniques on page 80 Element Lists on page 191 Data Tree on page 85 Mini View on page 93 Step Notes on page 94 iy ce EDS SEM The Business of Science Why Are Specimen Coated Samples are sometimes coated with a thin conductive layer prior to observation in the SEM to ensure that there is a good electrical path to ground This prevents non con ducting specimens as well as the oxides which are present on the surface of many samples from charging under
126. In the Auto mode the software checks for the accelerating voltage set on the microscope and selects a suitable energy range in the software Process Time Select the Process Time from the drop down list of Process Times Default and 1 to 6 The Proc ess time is the length of time spent reducing noise from the X ray signal coming from the EDS detector during processing By selecting different Process times it is possible to reduce dif fering amounts of noise The longer the Process time the lower the noise If noise is minimized the resolution of the peak displayed in the spectrum is improved the peaks are narrower and it becomes easier to resolve the peak from another peak that may be close by in energy If Default is selected the Process Time is automatically set to a suitable value Post Acquisition Image If this option is selected a new scan of the electron image with the current settings after the map Is finished can be acquired This can be used for checking any drift of the specimen Exporting Unprocessed Patterns Storing EBSD patterns without solving You have the option to store EBSP patterns and solve them later using the reanalysis tools Inthe Acquire Map Data toolbar click Settings Inthe dialog select Store Patterns At Storage Conditions select All Patterns without Solving 1 2 3 4 Select a storage format 5 Close the Settings dialog 6 In the toolbar click Start 459 Map da
127. Is described here Acquire and Confirm 2 222 2202 2 2 cece cece e cece ccc ceee eee ceeee 361 360 EDS TEM The Business of Science Acquire and Confirm Acquire and Confirm In Acquire and Confirm step four operations are combined into one window Acquire and Confirm is the main step of the Point amp ID Navigator in the Custom mode It is aimed for users who do not require any guidance during their analyses The workspace is divided into four quadrants Each quadrant represents an application For example Scan Image is located in the top left quadrant Acquire Spectra in the top right quadrant Quant Results in the bot tom left quadrant and Confirm Elements in the bottom right quadrant Press the relevant button in the toolbar from the view in any quadrant To re dock the free floating window back into the main application window press Ea Each application has identical functionality as its counterpart in the Guided Navigator To get help on each application follow the links below Scan Image on page 418 Acquire Spectra on page 313 Confirm Elements on page 330 36L Map Guided ccc In the Guided mode the Map navigator has the four steps The Describe Specimen and Scan Image steps are covered in the earlier section The steps which are unique to this navigator are described here Acquire Map Data 2 2 2 022 2occ ieee eee eee cece eee eee 363 Construct Maps
128. Map that you entered are selected by the maximum intensity Smoothing Level The maps may contain a lot of statistical noise if there is not sufficient data The noise can mask the distribution of elements in the maps You can filter out some of this noise by 210 EDS SEM The Business of Science applying Smoothing Level This operation applies a lowpass filter to an image to smooth the data If you are using TruMap it might be more effective to use binning Smoothing Level 3X3 The lowpass filter uses the following 3x3 kernel 1 9 1 9 1 9 1 9 1 9 1 9 1 9 1 9 1 9 Smoothing Level 5x5 The lowpass filter uses the following 5x5 kernel 1 25 1 25 1 25 1 25 1 25 1 25 1 25 1 25 1 25 1 25 1 25 1 25 1 25 1 25 1 25 1 25 1 25 1 25 1 25 1 25 1 25 1 25 1 25 1 25 1 25 ACB while acquiring Check this option if you wish to apply automatic brightness or automatic gamma to maps dur ing acquisition depending on your pre selection of Auto Brightness or Auto Gamma See also Acquire Map Data Settings below Context Menu Map Viewer on page 223 How binning affects the quality of your data on page 373 Layer modes in the interactive map display on page 216 Acquire Map Data Settings The settings cog is located near the top of the Acquire Map Data screen Clicking on it with the mouse displays the available settings 211 t Settings EDS Acquire Map Data Settings x Resolution 296 Acquisition Time
129. Pole Figure Inverse pole figures represent the orientation distribution of lattice planes in crystals and tex tures of materials You can construct an inverse pole figure after you have acquired map data 1 2 On the Orientation Information panel select the Pole Figure tab Expand the Construct Pole Figures Inverse Pole Figures tab and click the Inverse Pole Figure icon to open a settings dialog Select the values such as phases and planes then click OK to close the dialog The inverse pole figure appears in the Pole Figure tab This might take a few seconds You can watch its progress at the bottom of the tab The data appears in the Data Tree with the label that you gave in the settings dialog To see details about the inverse pole figure such as the number of projected points find the object in the Data Tree It has the label you gave in the settings dialog Right click and select Details If you have acquired EBSD data you can select the Show Orientation Information tool then click on a point on the map or image to display its solution unit cell orientation or corresponding orientation on the inverse pole figure in the Orien tation Information tabs If the data was acquired with stored EBSPs you can display the solution with the EBSP which helps you to interrogate the acquired data If the phase you selected to create the inverse pole figure matches the phase at the point you have selected the corresponding orientation ve
130. Profile All Settings gt ngs Binning Mode 2x2 Y Grex Si EBSD Phase Selection Settings Gaire i gt EBSD Solver Settings Exposure Time imst EBSD Specimen Orientation Settings EDS Acquire Line Data Settings E Auto Background EDS Acquire Map Data Settings Frame Averaging EDS Acquire Spectrum Settings Number of Frames EDS Element Settings EDS Peak Label Settings EDS SEM Quant Settings EDS TEM Quant Settings scan Image Settings Restore Defaults Cancel EXAMPLE Iam in charge of a service lab and have a number of users reporting to me We per form many different types of analysis that we carry out but do not have the luxury of assigning one person to do the same analysis all the time So it is important that we have a way of reducing the variability in analytical results between different users At the moment I make sure I check the users settings before they start 22 X O RD Getting started INSTRUMENTS The Business af Science For each analysis type all the relevant parameters can be saved in a profile along with per sonalized step notes to instruct the users on the analysis Subsequently anytime a user wishes to perform a particular type of analysis all they have to do is load the relevant profile and all the appropriate settings will be changed and associated step notes will be loaded Load User Profile Please select a profile from the list Application 1 Steel Analysis Cancel
131. Project menu is dis abled Saves the highlighted Project Makes a copy of the high lighted Project prompts to enter a name and then opens it in the data tree and closes the existing Project Menu Description Import INCA Imports an INCA Project adds Project it to the Project list if existing Projects contain data otherwise replaces an existing new Project Save As INCA Saves the highlighted project Project as an INCA Project Export to CHAN Exports the currently selected NEL5 Project EBSD data as a CHANNEL5 project CPR file or a Channel Text File CTF You may also include EBSD patterns as TIFF files This option is not available if you have stored EBSPs without solving Recent Projects Allows to load from the recent Projects that you have been working on Shuts down the application l f Getting started OXFORD The Business of Science View Menu Menu Description Data View It has the Current Site and Data Tree tabs Mini View It has various views such as a live spectrum image or acquisition progress bar Step Notes Provides a brief descrip tion of the main features of each screen Users can write and edit their standard operating procedures SOPs for future reference Application Available options are Zoom Level Largest Large Medium Small and Smallest Reset Layout Restores the default lay out on restarting the application Technique selector The te
132. RD INSTRUMENTS The Business af Science Measuring the distance between two points The distance between two points in the Linescan viewer can be measured using the Caliper tool 1 Select the tool from the toolbar on the left and move the mouse over a Linescan viewer stacked or tiled This cursor will track the mouse movement 2 Double click to set the first measurement point 3 Move the mouse to paint a region on the viewer which shows the distance between the two points This will update as the second cursor is moved 4 Double click to fix the position of the second cursor Bevel pa ee RR 900 1000 100 1700 1300 NOTE Unlike calipers on an image the linescan calipers are not saved with the data When you switch to a different tool the caliper information will disappear and will not reappear when you switch back A new region can be drawn by double clicking in the viewer at the new start point You can then define the extent of the measurement by placing the sec ond marker as described above To get rid of the region on the viewer you should switch to another tool on the toolbar In the Vertical Tiles view you can use the Caliper tool on individual linescans to display the dis tance between two points 3995 Viewing element counts and percentages 1 Select the Show data values tool from the toolbar on the left 2 Click on the line in the Linescan viewer A vertical cursor appears at
133. SD Channels Upper Left 3 Upper Right 3 p Image from a single FSD diode Lower Left 3 Lower Right 3 Side Left 3 Mixed image Side Right 3 SD Mixed Image 3 31 a Imported Image Any standard Windows Picture files can be imported into the Project for comparison or reporting The file formats available are JPG JPEG BMP PNG WDP GIF TIF and TIFF You can import an image using the context menu available from the Site Spectrum Spectra are acquired from the areas defined on an electron image Sum Spectra and Recon structed Spectra are shown under the Map in the Data Tree You will see the following items in the Data Tree if you are acquiring element maps in the EDS application Data View Current Site Data Tree A oS d q Specimen 1 4 lt gt Site1 Electron Image 1 a Map Data 1 a EDS Data Map Sum Spectrum Mg Kal 2 Ti Kal Cr Kal Mn Kal amp EDS Layered Image 1 Map Data 7 EDS Data Map Sum Spectrum Mg Kal_2 Ti Kal Cr Kal Mn Kal EDS Layered Image 2 Z Mineral imported image Map Data Map Data is the container for a mapped area s in a Site It can hold EDS Data EBSD Data or both One Site can contain more than one Map Data items In the example above there are two items Map Data 1 and Map Data 2 EDS Data Nie y Getting started Oy 45O ND INSTRUMENTS The Business af Science EDS Data is the container for Map Sum Spectrum Reconstructed Spectra
134. SelectSecond mage None E E It has controls for starting and stopping the spectrum acquisition There is a Settings cog for selecting the acquisition parameters For details see Acquire Spectra Settings link below The toolbar located on the left side of the workspace has various tools for image and spec trum manipulation enhancement annotation and area selection For details see Acquire Spectra Toolbar topic from the link below There are manual and auto brightness contrast and color controls available for the image view You can use these controls to enhance and high light certain features in the image The Compare Spectra amp MiniQuant Results option is available in the top right corner of the Spectrum viewer You can compare the current spectrum with any other spectrum from an opened Project on the Data Tree Instant MiniQuant results can be viewed in a table or a bar chart See also How to acquire spectra on next page Modes of X ray spectrum acquisition on page 150 Acquire Spectra Toolbar on page 151 Acquire Spectra Settings on page 313 Context Menus Spectrum Viewer on page 321 Export Settings on page 132 Peak Labels on page 158 Element Lists on page 191 147 How to acquire spectra You can acquire a spectrum from the entire image a single point or area on an image You can also acquire spectra from multiple points and or areas on an image Tools are provided to specify points and areas on the i
135. Selects the color of the selected phase Max Reflectors Selects the maximum number of reflectors that you can specify Show Unit Cell Shows an image of the unit cell inside the sphere Use Perspective Makes the image appear three dimensional Use 4 Digit Indices Selects the 4 digit index notation Generally the 3 digit index notation is used 14 Getting started The A te one of Science i EBSD Image Viewer You can control the default display of the Electron Backscatter Diffraction EBSD image To temporarily change the current display right click it and use the context menu Field Description Band Mode Shows the bands as edges or center lines Sum Indices Shows only those indexes where the sum of the indices does not exceed the number you enter here For exam ple if the value entered is three indices such as 100 and 111 may be labeled if displayed on the sim ulation However indices whose sum is greater than 3 will not be shown The value entered must be between 1 and 20 Min Intensity Determines how many bands are shown in the simulation A value of 0 shows all bands A value of 15 shows only those bands with an intensity greater than 15 The value must be between 0 and 100 Extend Bands Shows the bands extended beyond the band detection area Use 4 Digit Indices Selects the 4 digit index notation Generally the 3 digit index notation is used Display Simulation Shows a simulation of the
136. Series Specify Energy Window Lower Energy keV 0 071 Upper Energy keV 0 146 Update linescan with changes The default settings are automatic X ray line series and energy window width selec tion 256 OX FO RD EDS SEM INSTRUMENTS The Business of Science 2 To manually define the width of the energy window check the Specify Energy Win dow option Enter the values for Lower Energy keV and Upper Energy keV and m Update linescan with changes press 3 To manually select the X ray line for an element linescan check the Specify Line Series option Select the line from the Line Series drop down list and press Update linescan with changes d Linescans Display There are three different display options available from the controls near the top right corner of the Construct Linescans screen Display image full screen Display linescans and image Display linescans full screen See Also How binning affects the quality of your data on page 373 257 Linescan Custom In the Custom Mode the Linescan navigator has two steps The Describe Specimen step is explained in the earlier section The new step is described below Acquire and Construct Linescans 22 022 222 02e eee 259 258 EDS SEM Oy 45O ND INSTRUMENTS The Business of Science Acquire and Construct Linescans Acquire amd Construct The three com
137. Some options are available only if the required drop down list l l l diodes are installed and configured FSD only FSD Z Contrast uses upper and side FSD detector channel images Select this mode if you are inter ested in seeing density atomic Z contrast signal FSD Topo Orientation uses lower FSD detector chan nel images Select this mode if you are interested in seeing orientation contrast signal Custom include and exclude FSD detector channel images of your choice When you select either of the first two modes the soft ware automatically uses the FSD diode channels asso ciated with that mode For example FSD Z mixing mode uses the upper and side FSD diode channels The FSD Topo Orientation mixing mode always uses the lower FSD diode channels Custom mode allows you to mix any FSD diode channels Select Second Image Selects further images to compare with the electron images for example a forward scattered electron image This control is available only when the map dis play is for an image only Fm sz C Sets the number of images per row in the Standard and Interactive displays FSD only Offers a choice of image display ESD onl Standard you can add individual images or remove omy them from the mixed image Interactive similar to Standard You can also change the weighting and color contributed by each image Summary similar to Interactive and in a more com pact display Er L
138. Specimen in the Data Tree and select Edit Notes to write or edit notes in any step of the Navigator See also Element Lists on page 191 Data Tree on page 85 Mini View on page 93 Step Notes on page 94 2 9 Describe Model T Describe Model In this step the specimen is described by a model defined by a multi layered structure on a substrate In order to setup the model you will need to know the sequence of layers and their constituent elements There are four simple steps to completing the model Defining the layers Defining the composition of each layer Defining the thickness of each layer WwW LY ea Defining the density of each layer 1 Defining the layers The Model area of the screen is used to define the number of layers and their order You are able to add new layers re order and delete existing layers or clear the model The Clear All button will remove all the layers leaving an empty Bulk entry Initially when you start to describe a new Model or when the Clear All button has been pressed the program will display a single Bulk layer When you add additional layers to the model the Bulk layer becomes a Substrate To add a layer to the structure 1 Press Add Above The Bulk layer changes to the Substrate layer The first layer will always be the Substrate layer 2 To define a layer on the substrate press Add Above This layer in the structure i
139. TEM Linescan Template Linescan Tiled Linescan Tiled A4 docx EDS SEM Analyzer Template Current Spectrum Current Spectrum A4 docx EDS TEM Analyzer Template Current Spectrum Current Spectrum Ad docx EBSD Phase ID Template Electron Image EBSD Point Electron Image PointAcquireAd docs EBSD Map Template Electron Image EBSD Maps Electron Image EBSD Maps A4 docx Other Templates Batch Template Electron Image Multiple Spectra Electron Image Multiple Spectra Ad docd Cancel male 2 Click one of the tabs and change the settings as required Many preferences are available 3 After you change a setting click Save When you have finished your changes click Close Auto Save The software can automatically save the data in your current project at regular intervals If the computer or software fails suddenly you lose only a few minutes of your most recent work Save project When selected enable Auto Save after elapsed time Save every Sets the number of minutes that will elapse between each automatic save A suitable time is 10 minutes To save data at any time click the File menu then click Save EBSD 3D Phase Viewer You can control the default display of the 3D Phase viewer To temporarily change the current display right click it and use the context menu Show reflectors Shows the reflectors as solid lines edge lines center lines or shows no reflectors Unit Cell Color
140. Until Stopped Fixed Duration Frame Count 1 Energy Range keV Number of Channels 2048 Process Time Default Pixel Dwell Time ps 100 Frame Live Time s 5 Resolution You can set the resolution of your maps by choosing the number of pixels in the X dimension over which the beam scans The number of pixels in the Y dimension will depend on the aspect ratio of your microscope image If you are collecting X ray data from the entire image using the number of pixels used will be the number set in the map resolution option If you define an area using the rectangle Ellipse or Freehand tool X ray data will be collected from only this defined area with a proportional number of pixels Acquisition Time There are two options available for maps acquisition time Until Stopped If you choose this option the system will carry on acquiring data until you stop it Fixed Duration You can choose number of frames you wish to acquire by entering the number in the Frame Count dialog Number of Channels Select the number of channels from the drop down list of 1024 and 2048 with which you dis play the spectrum The number of eV channel will depend on both the energy range and the number of channels you select ole s EDS SEM The Business of Science Energy Number of eV channel Range keV Channels In the Auto mode the system checks for the energy range selected and sets the appropriate number of channels E
141. V in the window Normalize Spectra Region You have the current spectrum in the spectrum viewer m Select the second spectrum using the Compare drop down The second spectrum is overlaid on the current spectrum a Select the Normalize Spectra Region option from the toolbar The cursor turns into a crosshair a Click in the spectrum viewer to select the start point of the energy window A default window Is displayed about this point Drag the mouse to define your win dow and then release it A window will be drawn between the first point and the end point where you release the mouse Both spectra are scaled along the Y axis to the average value usually cps eV in the window Annotations Five tools available to add annotations on the current spectrum and the image are Caliper Angle Text Rectangle and Ellipse Select the tool by clicking on it and then click on the spec trum image to add annotation For example to add text select the Text annotation tool click on the spectrum where you wish to enter the text and then start typing the text To delete annotation double click on it to select it and then press the Delete key on the keyboard 100 EDS SEM OXF INSTRUMENTS The Business af Science Show Data Values With this tool you can view the Energy keV and counts in any channel of the spectrum Simply select the Show Data Values tool from the toolbar and then hover on spectrum The values will be disp
142. Viewer SEM Magnification 100 x l SEM High Voltage 20 00 kV PA ee Ewe SEM Working Distance 10 00 mm Stage X 0 00 mm Stage Y 0 00 mm EDS Linescan Viewer Stage Z 10 00 mm Stage Rotation 0 00 9 Stage Tilt 0 009 Image Viewer Specimen Tilt 0 00 AutoLock Status Off INCA Image Export EDS Input Rate 75981 cps EDS Output Rate 29981 cps EDS Dead Time 359 Status Bar EDS Process Time A EBSD Detector Insertion Distance 0 0 mm Welcome Screen EBSD Detector Signal Strength 0 0 EBSD Detector Note Level 0 0 SSS EDS Layered Image Settings EDS Spectrum Viewer E Reports E AEEA SSS aa Check the relevant check boxes to make your selection and press the Save button The selected parameters will be displayed in the Status Bar Ty You can access the Microscope Control by pressing located on the right end of the Status Bar 20 OXFORD INSTRUMENTS The Business of Science See Also Microscope control on page 493 Microscope Parameters on page 496 Getting started 21 User Profile A user Profile contains all the settings needed to reproduce analytical results obtained ona previous date or by another user The User Profile dialog is launched from the Tools menu on the main application menu bar To show only the settings for your type of analysis select from the drop down list in the top right corner For example change All Settings to EBSD Settings User Profile
143. Viewing element counts and percentages 1 Select the Show data values tool from the toolbar on the left 2 Click on the line in the Linescan viewer A vertical cursor appears at that location and displays the value for each element in that location For example If no sigma threshold is applied to TruLine processing some values might be negative To see the sigma threshold setting go to the Tools menu select User Profile and then the EDS Ele ment Settings tab 246 EDS SEM Oy 45O ND INSTRUMENTS The Business af Science Comparing element quantities The Normalize Y Axis option is available on the context menu of the Linescan viewer when in Stacked view It allows you to compare linescans with very different maximum count rates and is useful in QuantLine displays The maxima of linescans are scaled to the full height of the viewer It allows you to view the details of the minima of linescans with low count rate Note that there is no Y axis on the normalized linescans because the absolute scale is mean ingless 247 Smoothing the linescans The Smoothing Factor option is available from the Linescan viewer settings It allows you to smooth the linescans after normalization for visual clarity as demonstrated in the screen shots All Elements Ti kal Cr Kal 18000 a Fe Kool 16000 Al Kol 14000 Br Leal 7 N Kal 13000 E 0 Kor i mal liu WWT F Kol 2 10000 ai i
144. a Spectra Maps Linescans To compare quant results from two spectra select Comparison of Results Two Spectra template Then select the comparison spectrum from the Compare option in the Mini Quant and Compare option The compare spectrum will be overlaid on the current spectrum in the Spectrum Viewer The quant results will be displayed in the table below Ifyou wish to change the Quant Settings press the Settings button to display the Apply and Save Quant Settings dialog Make the changes and press The recal culated results will be displayed Alternatively make the changes to the quant set I tings and press Press the Close button to close the Quant Settings dialog Then press the Requantify button to display the recalculated results Quant Results Details You can see the settings used for calculating the composition in the Quant Results Details list box Parameter Description Label Spectrum Label E g Spectrum 1 Element List Type Current Spectrum Fixed List or Combined List 356 The Business of Science Parameter Processing Options Ratio Standard Element Ratio Standard Line Specimen Thickness Specimen Density Automatic Line Selection Thresholding Deconvolution Elements Pulse Pile Up Correction Detector File Efficiency EDS TEM Description All Elements or Oxygen by Stoichiometry Silicon K Series x nm X g cm Enabled or Disabl
145. a single workspace called Acquire and Confirm It offers the convenience of working in one window without hav ing to move away from it for acquiring a spectrum and obtaining the quant results You can choose which component you wish to display in the workspace by pressing the rel evant button in the toolbar from the view You can toggle to switch on off a component 7 Press B un dock a component as a free floating window located in the top right corner of the view Press to switch it into a full screen view E To re dock the free floating window back into the main workspace press Each component has identical functionality as its counterpart in the Guided Navigator To get help on each application follow the links below Acquire Spectra on page 96 Confirm Elements on page 353 Calculate Composition on page 185 123 Point amp ID Guided Point amp ID is an image centric application that requires the acquisition of an electron image prior to X ray spectra acquisition There are two modes of operation Guided and Custom In the Guided mode the Point amp ID navigator has six steps Describe Specimen and Compare Spectra are explained in the earlier section The steps which are unique to Point amp ID Guided are explained here Scan Image fe epee hison anal andes tae gs te ted oi nents oes 125 Acquire Spectra t opie dia sie teonag at ewseicteetciekaeamenedeandecseapeseeiace 146 C
146. a spectrum from the Data Tree in order to use it as a template Note that the values for the tilt elevation and azimuth angles displayed are of the template spec trum and are not editable 3 The livetime and the beam current factor are user selectable You can change these settings to find the optimum conditions Note that the calculated count rate Is a result of the spectrum simulation and is not directly editable 4 The accelerating voltage and acquisition range are taken from the template spec trum in the data tree but can be changed in order to explore how the spectrum depends on the accelerating voltage used 5 You may add the simulated spectrum to the Data Tree by pressing the Add Spec trum button Setting up a model Set up a model of your specimen by including all of the layers and the substrate of the spec imen you want to simulate This may be done either by using the Describe Model step or the interface provided in the Simulate Spectra step Once you are satisfied with the model you may save it by pressing the Save button This will ensure that your model is saved in the User Profile It should be noted that if you are generating a new model all values for the thickness and the concentration are set to fixed by default You may import a previously defined model tfe or tff files by pressing the import button or export the current model by pressing the Export button to share the model between sys 296 Lay
147. a spectrum full screen Acquisition Toolbar There is an acquisition toolbar near the top of the workspace Acquire Spectrum gt START STOP settings Select Second Image None It has controls for starting and stopping the spectrum acquisition There is also a Settings cog for selecting the acquisition parameters For details see Acquire Spectra Settings link below The toolbar located on the left side of the workspace has various tools for image and spec trum manipulation enhancement annotation and area selection For details see Acquire Spectra Toolbar topic from the link below Manual and Auto Color Contrast Brightness Gamma controls There are manual and automatic color contrast brightness and gamma controls available for the image view You can use these controls to enhance and high light certain features in the image For details of these controls see the link below Compare amp MiniQuant Results option The Compare Spectra amp MiniQuant Results options are available in the top right corner of the Spectrum viewer Instant MiniQuant results are displayed on completion of spectrum acquisition Results are separated into layers The layer thickness heads each line in the dis play Elements are listed next to the layer heading along with either the Atomic or Weight Fraction value as selected from the MiniQuant Settings cog The substrate layer is displayed at the bottom of the list The composition will be displayed i
148. acked spectra view and test if they improve the overlay fit Show Theoretical Spectrum This tool calculates a full x ray spectrum from the analyzed composition This calculation includes the efficiency of excitation of all lines the effects of absorption and backscatter within the sample and calculates the relative intensity of both lines and bremsstrahlung back ground Although the theory is not perfect it normally predicts peaks and background within about 10 accuracy If elements have been misidentified or element composition ratios are incorrect then the Theoretical Spectrum will appear significantly different from the observed spectrum either in terms of peak intensities or background When the theoretical spectrum is a good match to the observed spectrum this provides useful confirmation that the analysis results are sensible Note that the Theoretical Spectrum is calculated assuming that the specimen is flat and homogeneous If the specimen shows a lot of topography or has composition that varies throughout the information volume then the calculation will not be relevant For example if a spectrum is obtained froma point that is not directly visible by the detector then the emitted x rays will be absorbed on their way to the detector by an unknown amount or unknown material so the overall effect cannot be predicted Show No Pulse Pile Up Correction This is a useful tool for showing the pile up peaks sum peaks that have been remov
149. acquisition Flashing blue LED Fault A fault has developed Red LED The Thermal control tab displays the current state of the vacuum in the chamber a Under Vacuum the chamber is under vacuum Vented The chamber has been vented Fault A fault has developed The Thermal control tab also displays the extended mode state Note The start button for spectrum acquisition is disabled if the detector is not cold or it is cooling down 487 e LN2 Detector The Detector Control has a number of tabs depending on the type of detector The tabs are described below Thermal The Thermal tab displays the LN2 status The liquid nitrogen level is ok The liquid nitrogen level is low In Air The liquid nitrogen sensor is exposed to the air Sensor missing The liquid nitrogen sensor is not plugged into the x stream If the LN2 level is low there will be an audible alarm You can silence the alarm for one hour by pressing the Mute button Position If the detector has a motorized slide the Detector Control will show the Position tab This tab shows the current slide state of the Si Li detector as shown in the table below State Description Fully Inserted The detector is fully inserted into the microscope chamber and ready for acquisition Fully Retracted The detector is fully retracted from the microscope chamber Indeterminate Position The detector is at some position in between the end stops Fault A fault has dev
150. active Summary Links images for manip ulation of all layers using the Pan or Zoom controls Unlinks images You can manipulate individual layers using Pan or Zoom controls Changes the brightness and contrast of the currently selected image or map Adds or removes a map in the layered image The Lay ered Image icon is in the top left hand corner of the map A symbol representing the map appears on the layered image 453 Minimizes a map The Mini mize icon icon is in the top right hand corner of each map This is useful if you have too many maps in view The map moves to the Mini mized Map tab below the displayed maps Deletes a map from the anal ysis completely This icon in the top right hand corner of each map Restores a minimized map to its normal size The mini mized maps are on the Mini mized Map tab below the displayed maps Map TruMap Sets the mapping mode for X ray Element Maps Automatically adds maps to the layered image This is the Autolayer feature Changes the brightness and contrast and gamma for all the maps Data from Map Acquisition Once data acquisition starts the Data Tree is populated with new items as shown below 454 ON INSTRUMENTS EBSD The Business af Science Map Data 2 a P EBSD Data Band Contrast 2 P Phase Color 2 p Euler Color 2 PF IPF X Color 2 PF IPF Y Color 2 ma IPFZ Color EBSD Layered Image 2 a
151. age select the appropriate tool from the toolbar on the left side of the screen For details see How to acquire spectra on page 148 For details of spectrum manipulation and annotation see Acquire Spectra Toolbar on page 151 You can see your MiniQuant results in a table or a bar chart during analysis Real time Compare and instant MiniQuant options are available in the Acquire Spectra Confirm Elements and Calculate Composition Comparison of Results Two Spectra template steps You can compare your current spectrum to a control spectrum dur ing acquisition For further details see Compare Spectra amp MiniQuant Results on page 195 73 Note You can navigate to the Confirm Elements step from a quick link Peaks in the spectrum are identified and labeled automatically using the AutoID and Pre defined elements lists If too many peaks are close together you can move the peak labels for clarity Select the Annotation tool available in the toolbar on the left of user interface in Acquire Spectra and Confirm Elements steps Click on the label to select it and then drag it to a new position For details of configuring peak labels see Peak Labels on page 158 Navigate to the Confirm Elements step to manually confirm the elements identified by AutolD if selected Extensive tools including Show Markers Show Peak Shapes Show Fitted Spectrum Show Theoretical Spectrum from the Settings and Show Candidate Elements from the toolbar o
152. al Elements identified manually If the Pre defined Elements have been specified these will be included for identifying and labeling peaks in the current spectrum automatically Note that the Identified Elements are saved in the Spectrum Perform Auto ID During Acquisition option is enabled by default and can be deactivate by un checking it in the Describe Specimen step as shown in the screen shot above You can then AutoID at any time by pressing the button Additional peaks in the spectrum can be identified manually by using the Show Candidate Elements tool in the Confirm Element step Click on the question mark icon to select the Show Candidate Element tool Position the cursor at the center of a peak by double clicking 163 with the mouse The list of elements spectra corresponding to the energy at the cursor is dis played in the panel on the right By highlighting an element in this list you will see the markers showing all the lines for this element Note that the Identified Elements will be quantified if you have selected the Current Spec trum or the Fixed List and Current Spectrum Element List in the Quant Settings in the Cal culate Composition step or EDS Quant Settings in the User Profile dialog Note EDS Quant Settings are available in the User Profile Dialog accessed from the Tools menu These settings are also available from the Calculate Composition step Fixed List The elements in the
153. al from the diode Opens a dialog where you can adjust the gain and offset of the signal from the diode This con trol is effective only while data is being acquired A Adjusts the level for the darkest and brightest parts of the image Offers a choice of color for the image 433 Control Description Context menus Right click the image to display context menus for copying exporting and printing images Exported data includes the mixed image and the images from each diode This data is not supported by some earlier versions of the soft ware Use the mouse wheel to zoom in and out of the image Minimized Images Any minimized images are stored on this tab which is below the displayed images Allows you to change the Brightness Contrast and Gamma for all the images The Auto Bright ness button optimizes the images to give the best Mixed Image The Auto Gamma button ena bles you to see all the image data including background noise FSD Control Dialog This dialog appears when you click FSD Settings in the Scan Image settings Here you can select the signals from preset combinations of diodes or make your own selec tion from any number of diodes to construct a forward scattered image The choices on the dialog depend on which diodes are fitted on the detector Use the following controls Control Description FSD Topo Orientation Uses the signals from the bottom two diodes to accentuate topog raphy
154. al spectrum and the fitted spectrum over the experimental spectrum or numerically by comparing predicted and measured k ratios and reviewing the sensitivity of the solutions to assumptions in the model or beam cur rent fluctuations Spectrum Overlays The options of theoretical and fitted spectrum overlays are available from the Settings cog Theoretical Spectrum Under Settings when you check the Show Theoretical Spectrum option a theo retical spectrum is overlaid on the experimental spectrum This option calculates a full X ray spectrum from the composition defined for the current model The calculation includes the efficiency of excitation of all X ray lines the effects of absorption and back scatter within the specimen and calculates the relative intensities of all lines in addition to the Bremsstrahlung background Although the theory is not perfect it normally pre dicts peaks and background within about 10 accuracy If any elements have been mis identified or the element composition ratios are incorrect the theoretical spectrum will appear significantly different from the experimental spectrum either in terms of peak intensities and or background When the theoretical spectrum is a good match to the experimental spectrum this pro vides useful confirmation that the analysis results are sensible a Fitted Spectrum Under Settings when you check the Show Fitted Spectrum option a fitted spectrum is overla
155. alent to white Starting from the original narrow range of signals the electronics has produced a wider range of signals which start at zero and reach the maximum The small range of grays is now fully black to white FSD diode controls You can generate a FSD mixed image by enabling the required diode detector channels For example you can choose the diode images to add to the mixed image the color for each image and their intensities The controls are around the image from each diode s432 EBSD The Business of Science Control Description Adds or removes an image in the mixed image Your changes to the number of images might affect the choices in the Mixing Mode drop down list Title States the source of the image such as the Top Left or Bottom Right diode x Minimizes an image This is useful if you have too many images in view The image moves to the Minimized Images tab below the displayed images The mixed image is not affected Deletes an image from the mixed image com pletely To restore a deleted image start a new image acquisition E Restores a minimized image to its normal size The minimized images are on the Minimized Images tab below the displayed images 100 J 100 Sets the weighting of the image within the mixed image For example 100 Uses the full signal from the diode 0 Does not use the signal from the diode 100 Uses a full inverted sign
156. also Acquire Map Data on page 363 Construct Maps on page 3 0 Acquire Map Data Settings on page 211 Context Menu Map Viewer on page 223 238 EDS SEM The Business of Science Linescan Guided In the Guided mode the Linescan navigator has four steps Describe Specimen Scan Image Acquire Line Data and Construct Linescans The two new steps are described here Acquiring linescans 0 22 0222 e eee eee eee cece ee cece eee eeeee 241 Displaying and manipulating linescans 22 243 Measuring the distance between two points 245 Viewing element counts and percentages 22 2 246 Comparing element quantities 22 2022 222222 e eee 247 Smoothing the linescans 22 02222 c cee e eee eee eee eee 248 Linescan Data 2 2 22 2 22 0 c occ cece cece eee eee eee e eens 249 Exporting the linescan data 222 0 2222 c eee eee eee eee eee 250 Extracting a single spectrum from the linescan 251 Extracting multiple spectra from the linescan 252 Construct Linescans 0 00000000000000 000000000000000 e ee eee 255 Acquire Line Data e a i Acquire Line Data In this step you can acquire element linescans along a line defined on the electron image or map The data can be processed in
157. alue in the Count Limit text box The default value is 500 000 Pulse Pile Up Correction Check Pulse Pileup Correction check box if you wish to automatically correct the spectrum for pulse pileup peaks Uncheck the box if you wish to disable this correction Pileup peaks can occur when a second pulse arrives and triggers the measuring system dur ing the time required to process a previous pulse When this happens neither pulse will appear in its correct position The result being a peak at a higher energy equivalent to the sum of the energy of the two photons The largest pileup peaks will be seen at twice the energy of the main peaks e g Fe Ka pile up peaks will be seen around 12 8 keV Notes The pileup correction algorithm assumes that the count rate at every energy is constant throughout the analysis period Therefore the correction works best when analysis is per formed on single pixels points or areas of same composition Bad results may be obtained if the beam is rastered over an area where composition is changing or if a spectrum is recon structed from a SmartMap over a region where the composition is changing Acquire Spectra Toolbar The Acquire Spectra screen has a toolbar on the left side of the workspace shown in the screen shot below 316 EDS TEM Oy 45O ND INSTRUMENTS The Business af Science Tools to pan normalize add annotations and show data values Drop downs with alternativ
158. am measurement 66 68 binning effect on maps 214 224 373 reduces noise 214 223 373 shortened linescans 215 224 373 C CHANNEL5 EBSD pattern data is not available 459 coating evaporation 80 specimens 79 techniques 80 color key 55 confidence factor 25 499 context menus Image Viewer Map Viewer Pole Figures report templates Spectrum Viewer CSO Sample Primary Coordinate system CS1 Data Acquisition Coordinate system Current Site D Data Tree linescans menus Phase Image phase maps Data View detector EBSD control EDS control drift correction see AutoLock E EBSD data folder EBSD detector control EBSP correcting distorted indexing of storing without solving EDS detector control electron images layer modes Energy Calibration evaporation for coating F F1 getting help File menu forward scatter electrons FSD data tree 500 144 157 223 471 50 103 321 415 415 29 30 85 249 399 38 33 89 229 380 28 489 484 133 35 9 489 440 416 459 484 216 66 306 80 61 7 129 130 422 424 130 424 31 87 The Business af Science diode controls gain and offset controls how to obtain good images optimize mixed image optimizing the mixed image FSE image collecting H help highlights remove after search images how to obtain a good FSD image INCA export image interface inverse pole figure IPF L la
159. an I use my single software on a different PC or Laptop Yes you can If you have your software installed on another computer you will need to Deac tivate the license on the existing computer and then Activate the license on the other com puter Transferring the Active license to the second PC does of course mean that your software will no longer run on the first Deactivated computer because you only have a sin gle license Each software platform has its own separate License Code so you will need to do this for each platform Can I transfer my single license between computers more than once Yes you can transfer Deactivate and Activate a license any number of times but remember you can only Activate a single license on one computer at a time Can I use my software on more than one PC or Laptop at the same time Although you can install your software on more than one computer at the same time if you have a single license you can only activate it on one of them at a time If you have a multiple licenses you can activate the license on as many computers as your license allows If you want to use your software on more computer than you currently have licenses for you can easily buy additional licenses as required from your representative I have forgotten the password What can I do If you cannot remember a password when re activating a license you can request a new pass word to be sent to the email address that was given during
160. and provided your License Code is valid an Unlock Code number will be returned to the Licence Manager that will unlock the soft ware you have purchased Once Activated you will not need to do this again unless you want to Deactivate a License Code Each software platform has its own separate License Code so you will need to do this for each platform My system computer does not have Internet access so how can I activate my License Code If your system does not have direct access to the Internet you can still Activate your License Code using any other computer with Internet access See NLS Getting Started Card and User Guide for details Can I install the software on more than one computer PC or Laptop at a time Yes you can The terms of the license allow you to install the software on any number of PCs within your organization but you will only be able to use the software on computers which have a valid License Code installed and Activated What is a single license Unless you specifically ordered multiple licenses when you purchased your system you will have a single licence which means you can Activate your software only on one computer at a time If you need to run the software on more computers you can Deactivate one computer and Activate another or you can buy additional licenses What is a multiple license If you purchased multiple licenses you will be able to run the software on the corresponding number of computers at th
161. and Custom In the Custom mode the Analyzer navigator has three steps The Describe Specimen and Compare Spectra are explained in the previous section The one new step is described below Acquire and Confirm 2 2222 2 222 c2c eee cece eee cceeccceeeceeeeeess 341 340 EDS TEM The Business of Science Acquire and Confirm Acquire and Confirm Acquire and Confirm is the main step of the Analyzer Navigator in the Custom mode Three components are available in the single workspace The Acquire Spectra component is located in the top half of the workspace Quant Results in the bottom left and Confirm Elements in the bottom right The three components are combined in the Custom mode to give you a single workspace called Acquire and Confirm It offers the convenience of working in one window without hav ing to move away from it for acquiring a spectrum and obtaining the quant results You can choose which component you wish to display in the workspace by pressing the rel evant button in the toolbar from the view You can toggle to switch on off a component 7 Press B un dock a component as a free floating window located in the top right corner of the view Press to switch it into a full screen view E To re dock the free floating window back into the main workspace press Each component has identical functionality as its counterpart in the Guided Navigator To get h
162. and click on the Standardize step your own standards database will be created At this stage your database will contain only the Factory Standardizations Once you have standardized entries your standards database will be modified accordingly To manage your Standardizations the following functions are provided Creating a new standardization file To create a new standardization file Press the Manage button in the Standardize screen and then select the Create File tab Select an existing file from the Factory Files or User Files This file will be used to pop ulate the entries in the new file Enter the name for the new file and press the Create button A new file will be created You can overwrite the existing entries in the new file with your own stand ardizations To use this new standardization file select it in the Quant Settings in the Calculate Compositions step for quantitative analysis Note The Factory Standardization file is available to all users of the system However files created by individual users are user specific Deleting a user standardization file Remember that you can not delete the Factory Standardization file User created files can be deleted To delete a User Standardization file 267 Select the Delete File option from the Manage Standardization dialog Select the standardization file to delete from the drop down list Press the Delete button The selected file will
163. and orientation FSD Z Contrast Uses the signals from the top two diodes to accentuate the atomic number contrast Custom Allows you to create any combination of signals using the controls labeled EO Uses the signal from the diode Uses an inverted signal from the diode 434 EBSD The Business af Science Control Description Does not use the signal from the diode Your selections are retained in your user profile 435 Optimize Pattern Optimize Pattem This step contains the necessary functions to allow optimal EBSP acquisition and processing Monitoring the EBSP The electron image shown in the top left quadrant is the image collected in the Scan Image step As you enter the Optimize Pattern Step the position beam tool is highlighted on the toolbar Positioning the beam around the image allows you to check the quality of the EBSPs from different points on the specimen The EBSP is shown in the top right quadrant unproc essed EBSP When the tool is selected the beam can be controlled by the mouse as well as by the keyboard Shift will give a coarse shift and Ctrl will give a fine shift with the arrow keys Alternatively press Center to position the beam at the center of the image Press the Off but ton to release the beam Adjusting the Camera Settings Select the binning and gain for the camera suitable for the analysis and then set the expo sure time to get suitable illumination Alte
164. aps on top of the electron image Viewing and Manipulating Maps You can choose how you wish to view your data Various tools are available to manipulate and view the X ray maps Map Size You can choose the number of maps per row using the slider bar for displaying maps you wish to view in the Standard and Interactive display mode EDE L Display Modes 208 EDS SEM Oy 45O ND INSTRUMENTS The Business of Science Maps can be viewed in three different display modes available from the drop down list on the Display toolbar Standard Interactive In the Interactive mode you can change the color of individual maps from the Hue drop down list The Layer Mode can also be chosen from Mix and Overlay modes available from the electron image Summary In the Summary view you see details of the energy window and X ray line used for each map in addition to other details such as Layer Name Source AutoID or User Map Color and if it is selected for the Layered Image See the screen shot below Map Color Energy Window keV Line Visible layer Ti Kal AutolD 444 4 58 Cr Kal AutolD 9 4 5 49 Min Kal AutolD 80 3 82 5 98 Er Lal 2 AutolD 143 1 53 Al Kol AutolD 210 144 1 54 Mg Kal_2 AutolD 0 21 130 le fel fel fe fe fe ie N Kol 2 AutolD 90 0 35 0 45 O Kal AutolD 0 48 0 57 le ie Electron Image 1 Link Unlink Press ES to link images for manipulation of all layers
165. are into the Com pare table spectrum Label Spectrum Color Line Thickness Project Path spectrum 1 r Normal Project 1 Specimen 1 Site 1 spectrum 2 2 Normal Project 1 Specimen 1 Srte 1 spectrum 3 Normal Project 1 Specimen 1 Srte 1 If you want to remove any spectra from the table highlight the spectrum and press Remove Spectrum You can choose which of the available spectra you wish all the others to be compared to by selecting your reference spectrum from the compare table and pressing Select Reference Spectrum Settings You can change the color of individual spectra by selecting the color from the drop down list in the compare table To change the line thickness of individual spectra select it from the Line Thickness drop down list in the Compare table To apply the chosen line thickness globally select it from the Compare Spectra Settings from near the top of the Compare viewer Normalize 358 EDS TEM OXFORD INSTRUMENTS The Business of Science Normalize is a useful function for comparing spectra acquired using different input X ray count rates such as spectra acquired with two different beam currents Note that you can normalize spectra using a point or a region Normalize Spectra Point e Select this option from the toolbar near the top left of the Compare Spectra screen e Double click in the spectrum to set a normalization point along the X axis e A window is d
166. as asegment within the sphere When you choose this display setting it is applied to all your inverse pole fig ures for Inverse Pole Figure only You can also select this option on the Preferences dialog on the Pole Figure tab Offers choices of output For example you can print the figure or send it by email Using the Settings option here you can change the size of the figure Details Shows details such as the number of projected points and the phase name 472 EBSD The Business af Science Phase D _ _ The Phase ID navigator has six steps Describe Specimen Scan Image and Optimize Pattern are described in the Map section Three steps which are unique to Phase ID are described in detail below Acquire Data 2 2 2 2 22 0000000000000000 0000000000000002 22222222 474 Search Phase _ 6 6 cece cee ence cece eee ee eee 477 Identify Phase __ 2 2 2 02 222 c cece cece cece eee ee cece cece eee ees 480 473 Acquire Data o Acquire Data The use of the EBSD to identify unknown phases in a material is called Phase Identification Phase ID For many years EBSD has been used to discriminate between several phases in a specimen using Phase discrimination either by analyzing single patterns from various phases or by automated mapping of such phases Phase ID takes this approach a step further by utilizing chemical analysis in conjunction with a crystallographic phase data
167. as shown in the screen shot below Map Data 1 a PEJ EBSD Data p Band Contrast 1 Phase Color 1 P Euler Color 1 IPF IPF X Color 1 IPF Y Color 1 IFF Z Color 1 EBSD Layered Image 1 IPF IPF These components are described briefly with their respective icons D Band Contrast Band Contrast is an EBSP quality number higher the number more contrast there is in the EBSP 2555 Phase Color This component colors the pixels in the map based on which phase was identified The color for each phase is defined in Phases for Acquisition tot Euler Color The Map component colors the map based on the Euler color scheme and will help to show different orientations within the map Euler 1 R Euler 2 G Euler 3 B IPF X Color IPF Y Color IPF Z Color The IPF color components color the pixels based on the orientation of the unit cell and chosen reference direction x y or z Note that the color key depends on the structure type so it is not always the easiest map to interpret EBSD Layered Image A Layered Image is a composite image created from electron and EBSD map images or ele ment maps if EDS is present as shown in the screenshot above Point Data In Phase ID a Point Data node appears in the Data tree when spectra and EBSP are acquired from the points defined on the image 36 Getting started OXF INSTRUMENTS The Business af Science Data View Current S
168. ase is a possible indication of a chemical compound The order of the phases The order of the phases depends on the distribution and quantity of each group of elements The first phases indicate large areas of closely grouped elements Later phases show smaller areas that are more thinly distributed for example 2 SiO shows one large area or a few large areas that contain Si and O a 24 SiO shows smaller and probably more scattered areas that contain Si and O 377 The number of phases You can display more or fewer phases by changing the analysis settings or by merging phases manually See Also Analyze Phases settings on page 381 Merging phases on the facing page 378 EDS TEM The Business of Science Merging phases To simplify the results of the phase analysis you can merge some phases The result is a new phase with a combined spectrum and fewer phases overall For example these phases have similar spectra and might be considered to be the same phase You can merge similar phases in several ways Seta higher Grouping Level to automatically combine any number of similar phases a Manually merge any two phases To manually merge two phases 1 In the phase maps select a phase 2 Right click and in the context menu select Merge into 3 Select the other phase from the list The first phase disappears The spectrum phase name and color of the second phase are updated to in
169. ate to the Acquire Spectra step Select the Point Tool from the toolbar on the left of the window Click on different locations on the image to define multiple points Spectrum acquisition starts from the first point as soon as you click on the image The rest of the points are queued up for acquisition The position of each point on the image is marked as a cross and it is labeled as Spectrum x 1 2 3 As spectra are being acquired they are added to the Data Tree just below the image they are acquired from Status of each point is color coded i e current point from which a spectrum is being acquired is yellow all queued up points are blue and post acquisition points are white Spectrum acquisition from an area Having acquired an image in the Scan Image step navigate to the Acquire Spectra step Select an area selection tool from the Rectangle Ellipse and Freehand in the toolbar on the left of the window Click and drag the mouse to outline a rectangular ellipsoid or irregular shaped area on the image with the Rectangle Ellipse or Freehand Tool respectively Spectrum acquisition starts from the defined area as soon as you release the mouse The position of the defined area is marked with the relevant shape and it is labeled as Spectrum 1 Spectrum 1 is added to the Data Tree just below the image it is acquired from Spectrum acquisition from multiple points and areas Having acquired an image in the Scan Image st
170. ation Select the Show Data Values tool from the toolbar and click anywhere on the image to display the Intensity value at that point FSE area optimization If an FSD system is currently fitted this tool is available It helps you to improve the bright ness and contrast of any area of the FSD mixed image i 1 ost L 131 Normally the software calculates optimized brightness and contrast values for the mixed image over the whole area Some areas of the image might be very dark or very light so that features within an area of interest might not be well defined 1 Select the rectangle tool from the toolbar 2 On the mixed image find the area of interest 3 Click and drag to form a rectangle around the area When you release the mouse button the software calculates new values of brightness and contrast then applies them to your area of interest If necessary you can repeat this step or reacquire the image and try again Export Settings In this window you can change the appearance of the image and then print it or send it by email for example This window appears when you right click an image or spectra to open the context menu and select Export then Settings Control Description Preview These two tabs show the Image you are now creating and the original image which you saw when you selected Export then Set tings Original Offers a choice of units such as inches or pixels so that you can corre
171. ault window is displayed about this point Drag the mouse to define your win dow and then release it A window will be drawn between the first point and the end point where you release the mouse Both spectra are scaled along the Y axis to the average value usually cps eV in the window Annotations Five tools available to add annotations on the current spectrum and the image are Caliper Angle Text Rectangle and Ellipse Select the tool by clicking on it and then click on the spec trum image to add annotation For example to add text select the Text annotation tool click on the spectrum where you wish to enter the text and then start typing the text To delete annotation double click on it to select it and then press the Delete key on the keyboard Spectrum Acquisition Tools There are four spectrum acquisition tools Point Rectangle Ellipse and Freehand Select a tool to acquire spectra from points and or regions on the image For details see Modes of X ray spectrum acquisition on page 150 For step by step advice on spectrum acquisition see How to acquire spectra on page 148 Spectrum Reconstruction Tools You can reconstruct spectra from SmartMaps using Point Rectangle Ellipse and Freehand tools These tools are enabled on map acquisition Show Data Values With this tool you can view the Energy keV and counts in any channel of the spectrum Simply select the Show Data Values tool from the toolbar and then hover on spectrum Th
172. ayed in the panel on the right By highlighting an element in this list you will see the markers showing all the lines for this element The profile of each candidate element is overlaid on the current spectrum The color of the profile is different from the current spectrum to enhance the display and assist you in iden tifying and confirming elements Spectrum Height This tool aids in the manipulation of the height of each candidate element spectrum using the slider bar _ L Display MiniQuant amp Compare Real time compare and instant MiniQuant options are available in Acquire Spectra Confirm Elements and Calculate Composition steps You can see results without having to move away from the acquisition mode You can also compare the current spectrum to a control spectrum during acquisition You can view MiniQuant results compared in a table or as a bar chart The element list is taken from the Quant Settings in the Calculate Composition step The default Element List is Current Spectrum Element Lists Any list of elements in the software can be split into the following three categories Pre defined Elements elements expected in specimen Identified Elements typically based on automatic peak identification Auto ID Fixed List used for Quantitative analysis Pre defined Elements You may have prior knowledge of your Specimen and know what elements to look for Examples I want to look for a particular li
173. bar and click anywhere on the image to display the Intensity value at that point FSE area optimization If an FSD system is currently fitted this tool is available It helps you to improve the bright ness and contrast of any area of the FSD mixed image oie os 1 ost Normally the software calculates optimized brightness and contrast values for the mixed image over the whole area Some areas of the image might be very dark or very light so that features within an area of interest might not be well defined 1 Select the rectangle tool from the toolbar 2 On the mixed image find the area of interest 3 Click and drag to forma rectangle around the area When you release the mouse button the software calculates new values of brightness and contrast then applies them to your area of interest If necessary you can repeat this step or reacquire the image and try again Configuration of diodes on the FSE detector The EBSD detector can accommodate up to six forescatter diodes around the phosphor screen The diodes can be positioned in a number of configurations because each diode can be removed and refitted A025 2 The diode positions provide different signals Upper positions above the phosphor density atomic number Z contrast signal Side positions coupled with the upper diodes to provide a stronger signal Lower positions under the phosphor screen orientation contrast signal The following example is f
174. base in order to produce a list of candidate phases These phases are then used to index the EBSP from the unknown phase The steps in a phase ID analysis are typically Locate a grain or particle of the unknown phase Forward Scattered imaging will help to locate areas of different phases Acquire both EDS and EBSD data simultaneously Determine the composition of the phase using EDS analysis Search a crystallographic phase database for all phases using composition ranges of the elements present Index the EBSP using the list of candidate phases Determine the identification of the unknown phase Data Acquisition In this step you can monitor both EBSD and EDS data coming from specific locations or col lect and store data from specific points on your specimen Acquire Data toolbar Depending on the focus of the mouse you can move the electron image Spectrum or Pattern using the Pan tool Use the wheel mouse to zoom in and out 474 EBSD To add text on your electron image select the Text annotation tool click on the object where you wish to enter the text and then start typing the text To delete annotation double click on it to select it and then press the Delete key on the key board To delete all annotations on the object choose Select All from the Annotations context menu on the image viewer and then press the Delete key on the keyboard Click on this icon to select the Point To
175. be deleted Note that this file will not be deleted if it has been selected for quant You will be warned about it when you press the Delete button Restoring standardization entries The Copy Entries option allows you to restore standardizations from the Factory File to a User File or from one User File to another User File Press the Manage button in the Standardize screen and then select the Copy Entries tab Select User or Factory Standardization File as the Source File Select your standardization file which contains the modified entries as the Des tination file Select the entry in the Factory Standardization file that you wish to restore by click Ing on it Then Press the Copy button to restore this entry across to your file The modified entry in your file will be overwritten with the Factory entry For copying multiple entries hold down the Ctrl key while selecting individual entries Create File Select source file and entries select destination file Delete File Factory files Quant Standardizations Quant Standardizations Jun 23 2011 Copy Entries User files Element Line Standard i Beryllium Ksenes Be Beryllium Ksenes Be Boron Ksenes BN Boron Ksenes BN i Carbon Ksenes C Vit Carbon Ksenes C Vit Eroen sens BN forn eane TEN er Oxygen Kseres SiO2 Yes Oxygen Kseries Si02 Yes Fluorine K seres CaF Yes Fluarine Ksenes CaF Yes l Meon K senes We fw Yes Neon Kk senes We v
176. beam current Acquisition Mode There are three options to terminate the acquisition Auto Live Time and Counts If Auto mode is selected acquisition continues until enough counts are collected in the spec trum for quantification You can choose to terminate acquisition at the end of a preset Live Time Enter the required time in seconds into the text box This is the time for which the system is processing counts into the spectrum The live time clock runs slower than the real time clock so that the acqui sition for 100 live seconds takes longer than 100 real seconds This time is extended to com pensate for the output rate being less than the input rate by the degree of Deadtime You can choose to terminate acquisition at the end of a preset number of counts Enter the value in the Count Limit text box The default value is 500 000 Pulse Pile Up Correction Check Pulse Pileup Correction check box if you wish to automatically correct the spectrum for pulse pileup peaks Uncheck the box if you wish to disable this correction Pileup peaks can occur when a second pulse arrives and triggers the measuring system dur ing the time required to process a previous pulse When this happens neither pulse will appear in its correct position The result being a peak at a higher energy equivalent to the sum of the energy of the two photons The largest pileup peaks will be seen at twice the energy of the main peaks e g Fe Ka pile up peaks
177. bility Selection Q Manual Auto maximum intensity Smoothing Level 1 NoSmocthing Ei ACB while acquiring Sort Order There are three different ways of sorting maps Alphabetically By atomic number By maximum intensity in map sorts on the value of the brightest pixel in cps Layer Visibility Selection You can choose how the visibility of layers selected in the layered image There are two options Manual and Automatic In the Manual mode you must select which X ray maps to be included in the layered image In the Automatic mode first N maps Number of Map that you entered are selected by the maximum intensity Smoothing Level The maps may contain a lot of statistical noise if there is not sufficient data The noise can mask the distribution of elements in the maps You can filter out some of this noise by 368 EDS TEM The Business of Science applying Smoothing Level This operation applies a lowpass filter to an image to smooth the data If you are using TruMap it might be more effective to use binning Smoothing Level 3X3 The lowpass filter uses the following 3x3 kernel 1 9 1 9 1 9 1 9 1 9 1 9 1 9 1 9 1 9 Smoothing Level 5x5 The lowpass filter uses the following 5x5 kernel 1 25 1 25 1 25 1 25 1 25 1 25 1 25 1 25 1 25 1 25 1 25 1 25 1 25 1 25 1 25 1 25 1 25 1 25 1 25 1 25 1 25 1 25 1 25 1 25 1 25 ACB while acquiring Check this option if you wish to apply automatic brightness
178. but slower indexing 448 O45 OND Paap INSTRUMENTS The Business of Science Use Advanced Fit Improves the angular accuracy of the indexing procedure but significantly slows down the indexing process Select an Advanced Fit Level 1 is low 4 is high Advanced Fit goes back to the full EBSP and optimizes the solution fit For standard use do not select Advanced Fit Band Detection Area X and Shows the X and Y coordinates of Band Detection Area Y the center of the Band Detection Area To move the area select the Band Detection Area tool on the Optimize Solver toolbar and drag the displayed area with your mouse As the area moves the coordinates change automatically Alternatively you can type the coor dinates here Band Detection Area Shows the radius To resize the area Radius select the Band Detection Area tool on the Optimize Solver toolbar and drag the displayed perimeter with your mouse Alternatively you can type the radius here Apply Refinement Applies a previous refinement to the solver 449 Acquire Map Data f Acquire Map Data A Map is a regularly spaced grid of automatically acquired and solved EBSPs In this step you can setup acquisition of EBSD or combined EBSD amp EDS data from either the full area or a selected area Generally candidate phases are selected before collecting data This enables EBSPs to be solved during acquisition However you may choo
179. by default consists of the electron image and the Phase Color Map if you have more than one phase However you can change this configuration If you have only one phase the IPF Z is shown You can manipulate the layered image in several ways You can add or remove a layer from the layered Image minimize some maps or delete a map from the analysis completely In the case of EDS if you remove an X ray map this element will not be identified automatically by AutoID and will be excluded from the current analysis If an element is present in a specimen deleting or excluding it will affect the TruMap results 452 EBSD The Business of Science You can choose the color for your maps adjust intensities and decide which maps to add to the layered image The AutoLayer feature automatically scales and colors all the maps and in the case of EDS selects the best maps to provide an effective color image that delineates regions of different composition Maps are auto matically corrected for brightness and those that show similar structure are assigned the same color Maps that are very noisy are shown in gray The most sig nificant map for each assigned color are added to the layered image Map Tools You can change the appearance of the maps and layered image with these tools Description Sets the number of maps per row in the Standard and Inter active displays Offers a choice of map dis play Standard m Inter
180. cal fluctuations can some times appear like a real peak When it is difficult to decide whether a peak is present or not the EDS SEM The Business of Science Context Menu Item smooth func tion sub stantially reduces the Statistical fluctuation so that any real peak becomes more visible Noise Peak Include in Shows the Scaling noise peak and includes its value when the context menu option Reset Scales is used Exclude Shows the from Scal noise peak ing but excludes its value when the context menu option Reset Scales is used Hides the noise peak Compare Spectra amp MiniQuant Results Real time Compare and instant MiniQuant options are available in the Acquire Spectra Con firm Elements and Calculate Composition Comparison of Results Two Spectra template steps User can see results without having to move away from the acquisition mode Using these options you can e See your results during analysis Compare your current spectrum to a control spectrum during acquisition a View MiniQuant results in a table or a bar chart Click in the top right corner of the Spectrum Viewer in Acquire Spectra Confirm Ele ments or the Calculate Composition window to access the Compare amp MiniQuant options it In the above example Spectrum 1 is the current spectrum and Spectrum 2 is the comparison spectrum You can select the comparison spectrum from a Project cur
181. cans 393 Measuring the distance between two points 395 Viewing element counts and percentages 396 Comparing element quantities 000 2200 0 200 2 397 Smoothing the linescans 000 022 e ee eee eee eee eee 398 LiINneS CaN Data seenen eea RAES 399 Exporting the linescan data 0 00 200 2222 e ee eee 400 Extracting a single spectrum from the linescan 401 Extracting multiple spectra from the linescan 402 Construct LinescanS acoro E AE SES 403 Linescan Custom 22 02 0000 2o cece ccc cee e ee cece eee eee ee eens 406 Acquire and Construct Linescans 2 2 22 407 EDS TEM In Optimize there is only one step Calibrate There is one calibration routine Energy Calibration Calibrate on next page 305 Calibrate Calibrate There is Energy Calibration routine available from the Calibrate screen Energy Calibration For accurate identification of peaks you need to perform the Energy Calibration Energy Cal ibration measures the shift in the position of the spectral peaks and resolution of the system As the system has very stable electronics you may only need to calibrate the system once in several months provided the environmental temperature of the laboratory is fairly stable A few degrees change in the environmental temperature can cause a small shift in the position of peaks The Ener
182. ch diode for optimal brightness and contrast The opti mized electron image then appears after a delay of a few seconds When you first start the software the Auto check box is already selected for you Software Tilt Correction Enables the use of imaging tilt correction This is an important function when working with tilted samples If no tilt correction is done images and areas will be distorted If the software tilt correction is enabled it will be possible to correct scanned images and areas based on information about the tilt angle and the scanning tilt axis Continuous Scan If the Continuous Scan option is checked you will see the image start to scan down the win dow and it will continue to refresh after each frame If there are any instabilities in your spec imen e g charging or drifting problems then these will be apparent as the image may shift slightly after each scan In order to stop the continuous scan press the Stop button e Click Stop once and the scan will stop when the current frame is complete e Click Stop twice and it will stop immediately If you navigate to a different step the scan will stop at the end of a frame Number of Frames Enter the number of times you wish the beam to scan the site of interest for image acqui sition 423 Frame Time secs The frame time is displayed in seconds The value of frame time depends on the resolution speed and mains synchronize if available FSD Contr
183. check box Show Markers Clicking on one of the elements in the confirmed elements list puts up the markers for that element Lines series are color coded K series lines are marked in red L series lines are marked in green and M series lines are marked in purple Show Peak Shapes Peak Shapes one for each line series for each element are fitted to the spectrum using the Filtered Least Squares FLS approach This effectively removes the effect of background and corrects for peak overlap The Fitted Spectrum shows the fitted peak shapes superimposed on a close approximation to the background and this makes it easy to see if a particular ele ment has been missed or a peak shape is a bad match to the observed peak shape s171 Show Fitted Spectrum This tool is very useful for checking for the presence of small amounts of elements whose peaks are heavily overlapped in the spectrum It overlays a fitted spectrum onto the current spectrum The shape of the fitted spectrum is based on the elements labeled in the current spectrum AutoID If any peaks are incorrectly labeled or any elements missed then the fitted spectrum will not overlay correctly on your current spectrum Use the Show Candidate Elements tool to identify elements on the part of the spectrum where the fitted spectrum and the current spectrum have their greatest dis crepancy Then add the possible elements identified manually by double clicking on them individually in the st
184. chniques available are EDS and EBSD Select the technique you wish to use by pressing the appropriate selector button on the top left of the main screen Tools Menu Accessible Theme Oxford Instruments Theme Light Blue Theme Blue Theme Languages Default English French German Russian Chinese Simplified Japanese User Profile Settings available to create a user profile are EDS Acquire Line Data Settings EDS Acquire Map Data Settings EDS Element Settings EDS Peak Label Setting EDS Quant Settings Scan Image Settings Specimen Tilt Settings 10 Getting started The Business of Science Menu Description Preferences Preferences are saved per user Make your selection for the fol lowing Auto Save Image Viewer INCA Image Export Reports Spectrum Viewer Status Bar Welcome Screen Status Mes Sages lt 1 lt Help Menu Menu Description 12 Show Help Home Page Show Step Help Show NanoAnalysis Advice Launch User Manual Launch NanoAnalysis Encyclopedia Oxford Instruments Web site About Launches the Help Viewer with table of contents in the left pane and useful links to internal and exter nal sites in the right pane Opens the Help Viewer Pressing F1 on the key board loads the help page relevant to the active step of the navi gator Opens links to How to topics Opens the user manual as a PDF file Opens the Encyclopedia in the Window
185. clude information from the first phase See Also Analyze Phases settings on page 381 Grouping Level 379 Phase maps in the Data Tree The EDS Data folder contains phase map data in a folder which by default is labeled as Phase Image where is an automatically increasing number For example lTi 2 AIMgO x 2 AIMgO 3 FeMntr The EDS Data container contains the Phase Image folder which contains all the phase maps The name of a phase map is composed of a number and its elements for example 2 AlMgO To rename the phase right click the icon and select Rename A spectrum extracted from one of the phases For details right click the icon See Also Data Tree on page 85 Analyze Phases on page 375 380 Or LOR EDS TEM INSTRUMENTS The Business of Science Analyze Phases settings The software processes data acquired from the maps according to the settings for Boundary Threshold and Grouping Level To see the settings click on the Settings button The default settings are stored in the User Profile Find Phases t Settings AutoPhaseMlap Settings settings Mode Default Custom Boundary Tolerance 3 0 Grouping Level 2 0 Boundary Tolerance Boundary tolerance controls the behavior at the boundaries of each phase Ifthe boundary tolerance is low each pixel in the phase represents a pure spec trum If a pixel has contributions from several phases it cannot be i
186. contain only the Factory standardizations Once you have standardized entries your standards database will be mod ified accordingly Standardize allows you to add your own standards blocks and enter compositions of all standards on each block You can standardize on any of the elements available in the stand ards Adding composition of standards You can build your standards database by adding blocks of standards and the compositions of individual standards on each block Note that if you wish to use pure element standards you do not need to add standards a Press Standardize on the Optimize navigator The Standardize screen is displayed Press Add to add a block in the Standards Compositions area Enter the name for the block and press OK Your block will appear in the Block list box Press Add to add a standard The following dialog is displayed O raa standard oe Name Pyrite Choose your composition type from the options below and then specify a chemical formula e g NaCl Total weight should be 100 5 00 Number of Atoms Weight Composition Fe Cancel 265 Enter name for the standard Enter composition of the standard by choosing either Number of Atoms or Weight When you know the chemical formula select the option Number of Atoms The formula is validated as you enter it If you enter it in a wrong format for example feS2 or FES2 it will not be accepted For Weight
187. ct the Fixed List and Current Spectrum option MiniQuant results table will clearly display which list is being used A lock icon will be dis played against the Fixed List elements as shown in the screen shot below Sum Spectrum Compare gn In this example Fe and Ti are selected in the Fixed List The rest of the elements in the chart results are from the Current Spectrum because the Element List selected for quantification was Fixed List and Current Spectrum Note that the Fixed List is saved in a User Profile See also Describe Specimen on page 76 Acquire Spectra on page 350 Confirm Elements on page 353 Calculate Composition on page 185 User Profile on page 22 165 Compare Spectra amp MiniQuant Results Real time Compare and instant MiniQuant options are available in the Acquire Spectra Con firm Elements and Calculate Composition Comparison of Results Two Spectra template steps User can see results without having to move away from the acquisition mode Using these options you can See your results during analysis Compare your current spectrum to a control spectrum during acquisition View MiniQuant results in a table or a bar chart 4 Click in the top right corner of the Spectrum Viewer in Acquire Spectra Confirm Ele ments or the Calculate Composition window to access the Compare amp MiniQuant options e In the above example Spectrum 1 is the curren
188. ctly size the image before you print it or add it to a web page Width Height Keep Here you can type the actual Aspect Ratio size of your image When Keep Aspect Ratio Is selected you need only change Width or Height to keep your image correctly proportioned Vertical Scale Type This drop down list is avail able for spectra only To display data that has a wide range select Log arithmic 132 OXFORD INSTRUMENTS The Business of Science Control Check boxes Print Setup Save As AutoLock EDS SEM Description Depending on the type of image several check boxes might appear Select the options to add extra infor mation to your image Changes the size of the image for easier viewing This does not affect the size of the image when printed Copies the image You can then for example paste the image into a Microsoft Word document Opens the standard Micro soft Windows printer dialog where you can print the image immediately or apply the settings to use later Immediately prints the Image using existing set tings for the printer Opens your email service if available and attaches the image to anew message Saves the image as a bitmap file which has a bmp file name extension AutoLock is designed to increase the stability of data acquisition on SEMs and TEMs where the image may shift This image shift can occur for a number of reasons such as sample move ment d
189. ctors blink on the inverse pole figure in a color that matches the phase To make further changes to the pole figure right click on the Pole Figure tab to open a context menu For example you can change the direction and print the fig ure Pole figure Settings dialog This dialog appears when you click the Pole Figure icon 469 The label appears later on the object in the Data Tree You can type your own text here Otherwise the text automatically con sists of words that describe your selections in this dialog Phase Select a phase from the drop down list radio buttons Select Direction or Plane Indices Select a 3 digit or 4 digit index nota tion then type the required numbers Use 4 Digit Indices l in each box You can also select this option on the Preferences dialog on the Pole Figure tab Hemisphere Select the hemisphere and Projection Plane Seoul ye ane Inverse Pole Figure Settings dialog This dialog appears when you click the Inverse Pole Figure icon The label appears later on the object in the Data Tree You can type your own text here Otherwise the text auto matically consists of words that describe your selections in this dialog Radio buttons X Y Select a direction such as X or type a custom direction with alpha and beta angles Folded When selected creates a folded inverse pole figure Other wise an extended 90 degree segment inverse pole figure is created
190. d P p jopa d a Tes ct Tool to show data values on an image or spectrum The Pan tool allows to expand the spectrum along the vertical axis and move the spectrum along the horizontal axis To expand the spectrum along the horizontal axis with Pan tool selected hold down the Ctrl key while dragging the spectrum with the left mouse Normalize Spectra You can normalize two spectra over a selected point or a region Normalize Spectra Point You have the current spectrum in the spectrum viewer Select the second spectrum using the Compare drop down The second spectrum is overlaid on the current spectrum Select the Normalize Spectra Point option from the toolbar The cursor turns into an up down arrow Double click in the spectrum to set a normalization point along the X axis A win dow is drawn on either side of this point Both the spectra are scaled along the Y axis to the average value usually cps eV in the window Normalize Spectra Region 152 EDS SEM Oy 45O ND INSTRUMENTS The Business of Science You have the current spectrum in the spectrum viewer Select the second spectrum using the Compare drop down The second spectrum is overlaid on the current spectrum a Select the Normalize Spectra Region option from the toolbar The cursor turns into a crosshair Click in the spectrum viewer to select the start point of the energy window A def
191. d Elements are saved with the current Specimen Changing the Predefined Elements will only update the Pre defined Elements in the current Specimen It will not update any existing Specimens in the Project Data View Current Site Data Tree Project 1 Specimen 1 Specimen 2 4 lt gt Site Electron Image 2 Spectrum 9 Spectrum 10 Spectrum 11 af ao 3 4 Site3 Electron Image 3 Spectrum 1 Spectrum 13 Spectrum 14 177 The current specimen is the one that you are presently analyzing processing the data from For example in the screen shot above Specimen 3 is the current specimen Spec imens 1 and 2 are the other specimens in the Project Identified Elements The Identified Elements will include a Any Pre defined Elements Elements identified by Auto ID a Any additional Elements identified manually If the Pre defined Elements have been specified these will be included for identifying and labeling peaks in the current spectrum automatically Note that the Identified Elements are saved in the Spectrum Perform Auto ID During Acquisition option is enabled by default and can be deactivate by un checking it in the Describe Specimen step as shown in the screen shot above You can then AutoID at any time by pressing the button Additional peaks in the spectrum can be identified manually by using the Show Candidate Elements tool in the Confirm Element step Click on the quest
192. d layer thickness are also calculated Note that if a particular spectrum has been previously quantified the existing results are displayed unless the Requantify button has been pressed Available templates Select the template that you wish to use For customizable templates you can select which data type you wish to show in the columns when you view the results Press Edit Columns to show the window where you can hide show such columns such as Density Thickness Weight Templates for Single Spectra Ifyou want to see a comprehensive set of results froma single spectrum choose the Full Results Table customizable Single Soectrum template The results are shown for the spectrum currently highlighted in the Data View Templates that show results for a single spectrum present each layer as a separate row You may decide what information to display in the columns by pressing the Edit Columns button Select the type of information to display in the Edit Columns window Templates for Multiple Spectra To populate a multiple spectra template hold the Ctrl key down while choosing spectra on the Data View and then press the Add Selected Spectra button at the bottom of the Data View window Templates that show results for multiple spectra present each spectrum in a sep arate row In a given row there are there are repeated sets of columns one set per layer This is followed by another set of columns which refe
193. d resolution should be found if there are peak overlaps When acquiring SmartMap data you should choose your Process Time carefully 1 You may have been working on a Specimen in either Analyzer or Point amp ID where you have setup your acquisition parameters to optimize your quantitative analysis If you now wish to acquire SmartMap data and you think you may wish to recon struct spectra from your SmartMap data and then quantify these spectra you s155 should maintain these acquisition parameters This means that you may have to acquire data with along Process Time to maximize resolution but limit the maximum acquisition rate 2 You may have been working in either Analyzer or Point amp ID and you want to view the distribution of elements whose main peaks do not overlap as a map or a lines can In this case you should use a shorter Process Time which will mean that you can work with higher acquisition rates and shorter acquisition times The choice of Proc ess Time will very much depend on your sample and what you wish to do with your SmartMap data once it has been acquired 3 If you have started your Project in Map and you are analyzing an unknown sample we recommend that you use a long Process Time in order that you do not miss any detail in your spectrum However if you only wish to map certain elements whose main lines do not overlap you can afford to shorten the Process Time and increase the acquisition rate by increasing the
194. d side of the interface then double click on a peak in the spectrum viewer The candidate elements are dis played in a stacked spectra view on the right hand side of the window you can dou ble click on any of these elements to add or remove it from the confirm elements list Lead Pb Lal Double click to add or remove element You can control what overlays you see in the Spectrum viewer via the Confirm Ele ments Settings These overlays can be very useful in helping you to interrogate com plex spectra View Settings E Show Markers HM Show Peak Shapes E Show Fitted Spectrum E Show Theoretical Spectrum E Show No Pulse Pile Up Correction 170 EDS SEM ON INSTRUMENTS The Business of Science Press Include Exclude once you are satisfied with the identification of each element to build your list of the confirmed elements See Also Confirm Elements Settings below Confirm Elements Tools on page 174 Element Lists on page 191 Peak Labels on page 158 Compare Spectra amp MiniQuant Results on page 195 Confirm Elements Settings To display the Confirm Elements Settings click on the cog icon near the top of the screen The various option available are shown in the screen shot here View Settings E Show Markers E Show Peak Shapes E Show Fitted Spectrum E Show Theoretical Spectrum M Show No Pulse Pile Up Correction To select any of these options simply check the associated
195. defined Elements Pre defined Elements in Specimen Load from Profi le Save to Profile Clear All Pm 5m Eu Np Pu Am Include l Perform Auto ID Dunng Acquisition Double click on the element symbols that you wish to include in the analysis All the included elements will be marked with the green color key in the periodic table To save the Pre s Save to Profile defined Elements in the current User Profile press It means when you load the User Profile next time these elements will be included in the analysis If you have already created a User Profile with the Pre defined Elements in the User Profile Load from Profile dialog press r Clear All Pressing will deselect the Pre defined Elements from the periodic table and they will not be included in the current analysis The peaks for the Pre defined Elements if included in the analysis are labeled in the Acquire Spectra step MiniQuant will display the quant results for these elements as Wt or a bar chart The Pre defined Elements will be marked as Pre defined in the Confirm Elements list box in the Confirm Elements Step There may be other elements in the Specimen which are identified by AutoID routine if the Perform AutoID during acquisition option has been checked in the User Profile dialog 74 C KO RD LayerProbe INSTRUMENTS The Business af Science Tip Right click on the Project or
196. dentified and appears black Ifthe boundary tolerance is high all pixels are placed in the phase that fits them most closely The spectra for each phase shows small contributions from adjacent phases Low setting of boundary tolerance High setting of boundary tolerance 381 Grouping Level Phase analysis identifies all the phases in the sample Grouping combines phases that are sim ilar and can create a smaller more manageable number of phases overall Ifthe grouping level is low a larger number of phases are displayed The later maps show phases that occupy small areas and might indicate trace compounds Ifthe grouping level is high a smaller number of phases are displayed The maps typ ically show a few large areas If the Grouping Level is too high areas that you consider as separate phases will be merged together To resolve this problem you can reduce the Grouping Level until all the expected phases are shown and then manually merge any phases that you prefer to analyze as a sin gle phase See Also Analyze Phases on page 375 User Profile on page 22 Merging phases on page 379 382 Ox Ze PlD EDS TEM INSTRUMENTS The Business of Science Analyze Phases toolbars These toolbars are available in the Analyze Phases step Map display tools These controls are above and below the phase maps Settings Description Displays the phase image or the phase maps or both TT Bm Sets
197. des hydrides to be present in your sample you should add these manually to the peri odic table You should also be aware of the limitations of your databases For example data base entries may include minor elements e g rare earth elements hydrous phases with OH2 or end members of solid solution series Even in steels databases will often include the Fe end member rather than including Cr Mn Al etc You should be aware of the difference in spatial resolution of the EBSD and EDS Techniques Particles lt 200nm across may give good EBSPs but the EDS signal will come mainly from the surrounding matrix The following options apply to all elements listed in the table Uncertainty The Uncertainty controls how large the error margins on the quantified EDS data should be The default for this parameter is 100 The default value is set high to ensure that phases are not missed during a search due to inaccuracies in the chemical information in the structural databases or errors related to quant on highly tilted samples Threshold The Threshold controls the minimum allowed percentage of any element to be auto matically included Note that 10 is the default value for this If the percentage found of the particular element is less than the threshold the element is optionally included during the search Search Condition These options apply to the individual entries in the table Include This means include this element a
198. dth of the energy window select the Specify Energy Win dow option Enter the values for Lower Energy keV and Upper Energy keV and a Update X ray map with changes press The map will be acquired using the defined window width TO manually select the X ray line for mapping an element select the Specify Line Series option Select the line from the Line Series drop down list and press 3 1 i Update X ray map with changes l l l 7 The map will be acquired using the specified X ray line Reconstruct spectra from Layered Image or Maps using Point Rectangle Ellipse and Freehand tools The spectrum reconstruction tools are available in the toolbar on the left of the workspace Select the spectrum reconstruction tool from the four available options Toolsto specify points and regions on an image for spectrum reconstruction a Click on any image and drag with the left mouse to select a region A reconstructed spectrum is displayed in the spectrum viewer and it is also added to the data tree m MiniQuant results of the reconstructed spectrum are displayed You can compare the sum spectrum and the reconstructed spectra To confirm the elemental composition of a phase you can navigate to the Confirm Elements step in the Point amp ID package from the link below the Layered Image Viewer For details refer to Online Help See Also AutoLayer on page 222 Context Menu Map Viewer on page
199. e Cie ci pe z 1 r z T t 1 7 1 1 7 7 1 r 7 T J Uae pe Par Lines Serbion ES Mages amp Lineseans See the link for details Report Results on page 44 General user interface enhancements Software is now fully 64 bit which means AZtec can a Utilize more of the host PCs RAM Handle larger data sets Software is now ideally placed to cope with the ever increas ing demands for more and more data acquisition and storage Run multiple memory hungry Programs simultaneously without compromising the performance Note It is important to note that the software will now not run on 32 bit operating system New navigator selectors More robust user friendly drop down selectors Future proof easily copes with any new additions of techniques or navigators Analyzer SEM EDS Batch export of data tree objects Multiple data objects images spectra IPF maps etc can now be batch exported as bmp gif joeg png tiff or wmp files OXFORD INSTRUMENTS The Business af science eat Sane lata Irma a Paint Orma Setien ERG ad Paint Croan Section a QF Spectre Mapa Lin Faini Cron a al Mog Disia 1 a H a Wap Sun ip 4 8 pect Y Debate fun Ar Dara Pernon Eor Data niy Set ds Print Emai What s New in Version 2 0 Multiple data tree images can be saved at the original resolution even if each image has a different resolution Delete
200. e You can add spectra from any Project Specimen and Site of Inter est from the Data tree into this table Select which spectra you wish to compare by selecting them individually from the Data Tree Press Add Selected Spectra This will add all the spectra you wish to compare into the Com pare table spectrum Label Spectrum Color Line Thickness Project Path spectrum 1 r Normal Project 1 Specimen 1 Site 1 spectrum 2 2 Normal Project 1 Specimen 1 Srte 1 spectrum 3 Normal Project 1 Specimen 1 Srte 1 If you want to remove any spectra from the table highlight the spectrum and press Remove Spectrum You can choose which of the available spectra you wish all the others to be compared to by selecting your reference spectrum from the compare table and pressing Select Reference Spectrum Settings You can change the color of individual spectra by selecting the color from the drop down list in the compare table To change the line thickness of individual spectra select it from the Line Thickness drop down list in the Compare table To apply the chosen line thickness globally select it from the Compare Spectra Settings from near the top of the Compare viewer Normalize 338 EDS TEM OXFORD INSTRUMENTS The Business of Science Normalize is a useful function for comparing spectra acquired using different input X ray count rates such as spectra acquired with two different beam curr
201. e values will be displayed as you move from channel to channel Acquisition and Settings Toolbar Near the top of the Acquire Spectra window there are buttons for starting and stopping acquisition as shown below Acquire Spectrum START m STOP Settings Select Second Image None 3 Press the Start button to acquire a spectrum from a point or region specified on the electron image There is also a Settings cog in the toolbar For details of settings see Acquire Spectra Set tings on page 313 153 You can choose to display two electron images SE BSE side by side by selecting the second image from the drop down list in the toolbar Images can be linked for manipulation using the Link button Acquire Spectra Settings The settings are described in detail below Energy Range keV Select a spectrum energy range from the available options of Auto 0 10 0 20 or 0 40 keV from the Energy Range drop down list An appropriate energy range should be selected in conjunction with the current microscope accelerating voltage If the accelerating voltage is above 10 kV in order to view lines which may be excited above 10 keV the 20 keV range should be chosen Below 10 kV it may be more appropriate to choose the 10 keV range since no lines above 10 keV will be excited In the Auto mode the system checks for the accelerating voltage set on the microscope and selects a suitable energy range in the software Number of Cha
202. e A mm 0 000 0 000 Stage Y mm 0 000 0 000 Stage Z mm 0 000 0 000 Stage Tilt deg 0 0 Stage Rotate deg 0 0 Stage Backlash Stage tilt To display or change the stage tilt value select the Stage tab on the Microscope Control win dow If your stage tilt is motorized the current value can be displayed and changed More com monly the stage tilt is not motorized but if you are working with tilted samples it is nec essary to enter the current tilt value If you are working with tilted specimens and you are going to use the spectrum for quantitative analysis it is important to enter the correct value since it is used by the quantitative analysis program to calculate the specimen geometry 494 Hardware Control Oy 45O ND INSTRUMENTS The Business of Science EBSD orientation data relies on knowing the sample tilt so if the stage tilt can not be read automatically then it must be entered manually in order for the orientation data to be cor rect See also Microscope Parameters on next page 495 Microscope Parameters Microscope Control reads and controls the microscope parameters Ensure that the values in the Microscope Control window correspond to the current microscope parameters You can change the values displayed by changing the appropriate controls on the microscope This will automatically update the displayed values in the Microscope Control window If microsco
203. e Linescan viewer from in the top right quad rant as the data is being acquired as shown in the next screen shot 407 STOP Settings Display Stacked Settings Electron Image 1 All Elements 16000 Pai Ti kal Cr Kal 12000 uh tt te nee Mn Kal Line Data 6 n ca ll a Fe Kol T i g000 a Mg Kal_ O Kal 4000 a A Kal an cial ah Wa 200 400 600 800 Minimised Lines Mode Selected Element Details In the bottom right quadrant you can define energy windows and configure X ray line series from Selected Element Details AutoID can be used for initial display You can add or remove elements as you wish using the periodic table Linescan Details seyd uawa papajas Clear All Spectrum Viewer 408 EDS TEM OXF INSTRUMENTS The Business of Science The spectrum is available in the bottom left quadrant You can view the Line Sum Spectrum and navigate to the Confirm Elements step from within this component to manually confirm elements Confirm Elements ns Line Sum Spectrum 4 La a I li e Y oll CL Ll Dose atounadaonaatlererloenadaang 0 2 4 6 keV 409 The Business af Science EBSD EBSD ERE e 200022 o cece eee eee ee eee eee 412 Describe Specimen 2 222 222 2222 cece eee eee eeecceeeeeees 413 Scan LAAYO CA 418 Optimize Pattern 2 0 2 022 cece eee eee eee eee ee eee 436 Optimize Solver
204. e Orientation Information panel select the Pole Figure tab 2 Expand the Construct Pole Figures Inverse Pole Figures tab and click the Pole Fig ure icon to open a settings dialog 3 Select the values such as phases and planes then click OK to close the dialog The pole figure appears in the Pole Figure tab This might take a few seconds You can watch its progress at the bottom of the tab 4 To see details about the pole figure such as the number of projected points find the object in the Data Tree It has the label you gave in the settings dialog Right click and select Details 468 ON EBSD INSTRUMENTS The Business of Science gt If you have acquired EBSD data you can select the Show Orientation Information tool then click on a point on the map or image to display its solution unit cell orientation or corresponding orientation on the pole figure in the Orientation Infor mation tabs If the data was acquired with stored EBSPs you can display the solu tion with the EBSP which helps you to interrogate the acquired data If the phase you selected to create the pole figure matches the phase at the point you have selected the corresponding orientation vectors blink on the pole figure in a color that matches the phase To make further changes to the pole figure right click on the Pole Figure tab to open a context menu For example you can change the direction and print the fig ure Creating an inverse
205. e Spectrum Coating Element Carbon spectrum Details Details Coating Thickness 15 nm Coating Density 2 25 gm Automatic Line Selection Enabled Copy Ifyou want to see a comprehensive set of results from a single spectrum then choose the Full Results Table customizable Single Soectrum template and which ever spectrum Is highlighted in the Data Tree will have its results shown in this tem plate To populate a multiple spectra template hold the Ctrl key down while choosing spectra on the Data Tree and then press the Add Selected Spectra button at the bottom of the Data Tree window 117 Data View Current Site Data Tree Mineral Sample d Map Data 1 VG Spectrum 2 GL Spectrum 4 Do Cp o TE Spectrum 7 D pp j Line Data 1 gt Site3 Add Selected Spectra Spectra Maps Linescans To compare quant results from two spectra select Comparison of Results Two Spectra template Then select the comparison spectrum from the Compare option in the Mini Quant and Compare option The compare spectrum will be overlaid on the current spectrum in the Spectrum Viewer The quant results will be displayed in the table below Ifyou wish to change the Quant Settings press the Settings button to display the Quant Settings dialog Apply the changes and close the dialog Press the Requantify button to display the recalculated results Quant Results Details You can see the settings
206. e Tilt Correction Continuous Scan Number of Frames Frame Time secs FSD Control a AutoLock Image Scan Size In general the resolution of an image or Image Scan Size is defined as the number of picture points or pixels along the x and y axes e g 256 x 256 512 x 512 or 1024 X 1024 The quality of the image improves as the resolution at which an image is acquired is increased However a microscope monitor CRT is usually a rectangular display rather than square so the res olution is displayed as a rectangle i e 256 x 200 in order to take into account the aspect ratio The y dimension is set at installation when imaging is calibrated It will vary with each system Select the Image Scan Size for image acquisition from the following drop down options avail able 64 128 256 512 1024 2048 4096 8192 Dwell Time ps Images can be acquired using different speeds The beam dwells on each pixel for a specified length of time while the signal is collected and then it moves to the next pixel So the speed at which an image is acquired depends on the dwell time 128 EDS SEM The Business of Science Speed Dwell time Fastest Fast Normal Medium Slow Slowest Mains Synchronize Selecting Mains Synchronize on the Image Setup window synchronizes the start of each scanned line to the mains supply This will help to reduce mains borne interference in the image Note that the acquisition time will b
207. e concentration of elements in a Specimen can be calculated In deter mining peak areas in spectra two problems arise A typical spectrum contains characteristic peaks which are superimposed on a slowly varying background which is noisy because of statistical variations This background contribution needs to be carefully subtracted from the spec trum The energy resolution imposes a limit on the separation of peaks Identification of peaks is generally not a problem but overlapping peaks require decon volution before being able to extract the true peak intensities relevant to the elements present in the Specimen 263 Once these intensities have been determined a comparison is then made with standards of known composition followed by application of matrix corrections before the concentration of each element can be determined What does standardization do In order to make a direct comparison between intensity and concentration a standard Spec imen is referred to in which the relationship between Istd and Cstd is accurately known where Istd is the intensity from the standard and Cstd is the concentration of the standard Once this is known this ratio can be used to determine the concentration of that element in an unknown Specimen Cspe since the intensity of the element in the Specimen Ispe can be measured Let Cxspe be the concentration of element X in the unknown Specimen and Ixspe be the intensity of the relevant p
208. e for optimal brightness and contrast The opti mized electron image then appears after a delay of a few seconds When you first start the software the Auto check box is already selected for you 129 Software Tilt Correction Enables the use of imaging tilt correction This is an important function when working with tilted samples If no tilt correction is done images and areas will be distorted If the software tilt correction is enabled it will be possible to correct scanned images and areas based on information about the tilt angle and the scanning tilt axis Continuous Scan If the Continuous Scan option is checked you will see the image start to scan down the win dow and it will continue to refresh after each frame If there are any instabilities in your spec imen e g charging or drifting problems then these will be apparent as the image may shift slightly after each scan In order to stop the continuous scan press the Stop button e Click Stop once and the scan will stop when the current frame is complete e Click Stop twice and it will stop immediately If you navigate to a different step the scan will stop at the end of a frame Number of Frames Enter the number of times you wish the beam to scan the site of interest for image acqui sition Frame Time secs The frame time is displayed in seconds The value of frame time depends on the resolution speed and mains synchronize if available FSD Control Thi
209. e four menu items for the Specimen Rename Delete Edit Notes and Details Site Rename allows to rename a Specimen Delete deletes the Specimen from the Project Edit notes opens a dialog for editing Specimen notes Details Opens a dialog showing the Specimen Label Specimen Orientation and Pre tilted Specimen Holder The Details dialog will also include the specimen coating information if you have selected it in the Describe Specimen step There are six menu items for the Site Rename Delete Import Image Batch Report Print and Email 38 Rename allows to rename a Site Delete deletes the Site from the Project Import Image imports any standard Windows picture file for comparison or report ing Batch Report this saves the Microsoft Word or Excel report of all the data in the Site It uses the report Batch Template selected in the Preferences dialog accessed from the Tools menu CYXHOIRD Fi Getting started INSTRUMENTS The Business of Science a Print this prints the Microsoft Word or Excel report of the data associated with the Site Email this helps to send the report via Email Electron Image The menu items are Rename renames the Electron Image Delete deletes the Electron Image Add to Layered Image adds an electron image to the current Layered Image Add to Image Viewer adds an electron image to the current FSD Mixed Image Save As Saves the current elect
210. e marginally longer than when mains synchronize is not selected Note that Mains Synchronize will only be visible if the appropriate hardware is installed Input Signal Select the signals from the detectors on the microscope For EDS secondary electron imaging is generally most appropriate if you are imaging a sam ple which has topography whereas backscattered imaging is a very useful means of iden tifying areas of different composition on flat samples Secondary electron imaging is the most common form of imaging and for a first look at your sample choose this mode If you are analyzing a flat polished sample and you can see weak contrast switch to back scattered imaging which will tend to enhance this contrast by showing up areas of different phases For EBSD Forward Scattered Imaging is often used Because of the high angle of tilt dictated by the collection geometry required for EBSD many electrons are scattered forward and down towards the bottom of the phosphor screen Using Forward Scattered Electron FSE imaging diffraction contrast is enhanced and the resultant signal makes the presence of individual grains easy to identify The forward scattered electron signal produced is therefore ideal for EBSD investigations However the user may use any electron signal as required for the reference image If you select the Auto checkbox before you start a new FSE acquisition the software auto matically adjusts the signal from each diod
211. e not been allocated a color to see if they show any features that are not obvious in the layered image Context Menu Map Viewer A number of useful shortcut menus available as right mouse click in the map viewer are shown in the table below Context Menu Item Reset Image Scale View Color Bar Scale Bar Export Save As Original Res olution Save As Copy Print Email Settings Details How binning affects the quality of your data As the electron beam scans a line or area of the specimen data is acquired from numerous points Inevitably the signal from each point includes some noise If data is not acquired for long enough the noise level will be high By combining signals from several neighboring points the binning technique produces an averaged signal which has less noise overall The effect is similar to collecting the original data at a lower resolution and a longer dwell time 223 You can select the binning factor from the drop down list below the map or linescan display Effect of binning on element maps A binning factor of four combines 16 adjacent pixels from each 4x4 square into one new pixel For example Binning is useful when you are using the TruMap mode for mapping because of the improved statistics Binning also enables AutoLayer to combine similar maps more suc cessfully because of the lower noise See also AutoLayer on page 222 Effect of binning on linescans
212. e only to the presence of this element Intensity corrections are calculated assuming the presence of this element The total from this type of analysis is always 100 This option can be used when analyzing a specimen in which a significant quantity of a light element which cannot be detected is known to be present This method can also be used in cases where an element for which no standard is available is present e Oxygen by Stoichiometry Use this option if you want the concentration of oxygen to be calculated assuming that it is bound by predefined stoichiometry to all the other analyzable elements The stoichiometry is defined by the valency of the oxygen ions and the valencies of other measured elements a Number of Ions Enter the number of oxygen ions that are combined stoichiometrically to the other elements The calculations are based on the number of oxygen ions and how many atoms there are in each unit cell a Valency When Oxygen by Stoichiometry is selected the option for choosing the valency for each ana lyzable element becomes available The most common value for the valency of the element is displayed when you click on an element symbol on the periodic table To use a different value enter the new value in the Valency text box Normalize Results When this option is selected the analytical total of an analysis carried out using All elements or Oxygen by Stoichiometry is forced to 100 Use of this needs care
213. e options Pan The Pan tool allows to expand the spectrum along the vertical axis and move the spectrum along the horizontal axis To expand the spectrum along the horizontal axis with Pan tool selected hold down the Ctrl key while dragging the spectrum with the left mouse Normalize Spectra You can normalize two spectra over a selected point or a region Normalize Spectra Point You have the current spectrum in the spectrum viewer Select the second spectrum using the Compare drop down The second spectrum is overlaid on the current spectrum a Select the Normalize Spectra Point option from the toolbar The cursor turns into an up down arrow Double click in the spectrum to set a normalization point along the X axis A win dow is drawn on either side of this point Both the spectra are scaled along the Y axis to the average value usually cps eV in the window Normalize Spectra Region You have the current spectrum in the spectrum viewer Select the second spectrum using the Compare drop down The second spectrum is overlaid on the current spectrum a Select the Normalize Spectra Region option from the toolbar The cursor turns into a crosshair Click in the spectrum viewer to select the start point of the energy window A default window is displayed about this point Drag the mouse to define your win dow and then release it A window will be drawn between the first point and the end point
214. e options are 64 to 2048 Scan Settings You need to specify the drift measurement interval the AutoLock mode and enable disable Use Predictive Correction Measurement Interval Here you can specify the interval in seconds between tracking images Drift correction is applied after each tracking image is collected For slow drift long intervals are acceptable For fast drift or for drift that changes direction frequently shorter intervals are more accurate but will slow down acquisition The default value is 30 seconds Use Automatic Measurement Interval If you select this option the program will determine the measurement interval for you The interval is adaptive as the speed of drift changes over time the measurement interval will be increased or decreased accordingly If Predictive Correction is also enabled the automatic measurement interval will adjust to improve the quality of the predictive correction AutoLock Mode There are two modes of operation In field and Extended field In field In this mode the scanned area field of view is viewed in full all the time It means that map ping or analysis is done on an area within this field It also means that the drift correction is applied within this field Digital Zoom is not available in this mode The In field mode is illus trated in the figure below Full field view The amount of drift correction that can be applied is shown by the arrows from the analysis ar
215. e same time For example if you purchased five licenses you can Activate the software on a maximum of five computers then if you try Activating a sixth com puter you will be advised that all of your licenses are in use Unless you specifically ordered multiple licenses when you purchased your system you will have a single licence which means your software can only be Activated on one computer at a time If you need to run the soft ware on more computers you can of course Deactivate one computer and Activate another or buy additional licenses I ordered multiple licenses so why have I only got one License Code The License Code contains details of the software you have purchased and are entitled to use and the number of licenses computers you are entitled to Activate at the same time So if you purchased five licenses you will only receive one License Code but it will allow you to Acti vate five computers at the same time using the same License Code 56 CYXHOIRD FI Getting started INSTRUMENTS The Business of Science What is a License Code A License Code is a unique 18 digit number which you will have received with your system It contains encrypted details of the software you have purchased including the modules func tionality and the number of licenses When this number is entered into the software Licence Manager and the code is Activated the software functionality you purchased and are entitled to use is unlocked C
216. e spectrum The template spectrum provides both microscope detector geometry information and detector characterization information 3 Define a set of accelerating voltages to use for the solubility calculation as well as the target count rate and spectrum Livetime Press Update 4 Decide whether to disallow any particular X ray lines for the solubility calculation by deselecting them under the relevant accelerating voltage 5 Press Calculate Solubility to perform the calculation When you press the Calculate Solubility button the inputs from the model are taken into consideration and are used to work out under which conditions the problem is soluble and those where it is insoluble for a set of predefined accelerating voltages It then suggests a set of analysis conditions to use Accelerating voltage kV The X ray lines to use for each element in the specimen The acquisition range 0 10 keV 0 20 keV or 0 40 keV In more detail the calculation takes into account how the intensity of the X ray lines vary with kV and it will calculate the relative statistical variation in all the determined unknowns At different kVs different lines K L M are excited the electron beam may not penetrate all the layers and some X ray lines may be absorbed on their way out to the detector The Cal culate Solubility procedure will try to find a kV where the problem is both soluble and invert ible and where best precision
217. e to set them to zero Thresholding may be applied so that results below the selected sigmas are set to zero Thresholding will also ensure that negative insignificant values which sometimes result from trace element analysis are set to zero To enable Threshold Quantitative Results check this option in the Quant Settings The default value for Sigma is 3 which represents 99 7 confidence level Apply and Save a Apply and Save If you make a change to the Quant Settings and press the settings are saved and the currently selected spectra are quantified The quant results are updated imme diately Save If you make a change to the Quant Settings and press saved to be used when you do quantification next time the new settings are 337 Compare Spectra Compare Spectra This step in both the Point amp ID and Analyzer Navigators allows you to compare spectra acquired from different sites of interest and specimens from the currently opened projects You can compare spectra acquired using different settings for example energy ranges 0 10 0 20 or 0 40 keV and number of channels 1024 2048 or 4096 Spectra associated with the current Site can be added to the Compare table by holding down the control key and pressing Add Selected Spectra Note that if you have acquired the spec tra in Point amp ID the positions of all the spectra associated with the current Site of Interest are displayed on the imag
218. e used for each map in addition to other details such as Layer Name Source AutoID or User Map Color and if it is selected for the Layered Image See the screen shot below Map Color Energy Window keV Line Visible layer Ti Kal AutolD 444 4 58 Cr Kal AutolD 9 4 5 49 Min Kal AutolD 80 3 82 5 98 Er Lal 2 AutolD 143 1 53 Al Kol AutolD 210 144 1 54 Mg Kal_2 AutolD 0 21 130 le fel fel fe fe fe ie N Kol 2 AutolD 90 0 35 0 45 O Kal AutolD 0 48 0 57 le ie Electron Image 1 Link Unlink Press ES to link images for manipulation of all layers using the Pan or Zoom control Press trol to unlink images You can manipulate individual layers using Pan or Zoom con Brightness and Contrast You can adjust the brightness and contrast of the currently selected image or map Press on the Display toolbar to open the Brightness and Contrast dialog 36 7 Auto Brightness and Auto Gamma Using the Auto brightness and Gamma buttons on the bottom right hand corner of the Map display window allows you to change the Brightness Contrast and Gamma for all the maps The Auto Brightness button optimizes the maps to give the best Layered Image and the Auto Gamma enables you to see all the map data including background noise Element Maps View Settings You can manipulate and view the data by using various parameters available in the Settings H Settings Sort Order Maximum intensity Layer Visi
219. ea tracking area to the boundaries of the field of view Extended field 139 In this mode the maximum drift available is 50 2x zoom and 150 4x zoom Setting the zoom level reduces the size of the captured area If 2x zoom Is selected only the middle 50 of the field of view is captured The full field of view can be preserved by using the Maintain sub ject size option described below Maintain subject size You select an area you wish to map analyze on the microscope AutoLock preserves this area after the digital zoom is applied if you have checked the option Maintain subject size as illus trated in the screen shot below Before digital zoom is applied After digital Zoom Is applied This is done automatically by setting a new magnification on the microscope before acqui sition starts This value is determined by dividing the current magnification by 2 2x digital zoom or by 4 4x digital zoom if 25 is selected The Maintain subject size option is not available in the In field mode Note If the microscope does not have column control then Maintain subject size will not be available Use Predictive Correction If Use Predictive Correction is selected a correction is applied periodically at selected inter vals between tracking images It is a useful option if your sample has a fairly consistent amount of drift At the start two reference images are acquired You can define the interval be
220. eak from element X in the unknown Specimen All intensities are assumed to have been corrected for background The concentration of element X in the unknown Specimen can be approximated as Cxspe Cxstd Ixspe Ixstd and is often referred to as the Apparent concentration or the uncorrected concentration Once these Apparent concentrations have been determined the element weight percents are then calculated by applying a matrix correction to the measured intensity ratios These corrections attempt to account and correct for the effects of X rays traversing the Specimen matrix such as absorption of X rays in the material The ratio in value between the Apparent concentration and the true concentration is a meas ure of the matrix corrections which need to be included in the calculation However the need for the correction is minimized if the composition of the standard Specimen is as similar as possible to the composition of the unknown Specimen This simply means that the effect on the X ray intensity of X rays traversing the Specimen and standard is similar Since these matrix corrections can be calculated with only a certain degree of accuracy the choice of standard material is very important if the quantification is to be as accurate as possible Why Standardize The need to standardize depends very much on the level of accuracy you require from your analysis on any one material As a rule of thumb If you require accuracy such that t
221. ectra Letter docx To generate a Batch report at any time 1 On the Data Tree select one or more sites then right click and select Batch Report 2 Select a folder for your reports and click Select Folder One document is generated for each site The documents are named according to the project name the site name and the current date and time Compile a report on the fly You can prepare your report as you acquire data The image spectrum and map viewers have a range of context menus which allow you to export live or stored data You can copy images spectra or maps to the clipboard and paste them into Microsoft Word or Excel You can manipulate images spectra and maps using various settings such as width height aspect ratio and zoom before exporting to a third party reporting application You can email or print an image spectrum or map from the respective viewer See Also Context Menu Report Templates below Preferences on page 13 Changing the logo in your reports on the facing page Generating your own report template on the facing page Context Menu Report Templates After you select a template for a report you can change the magnification of the preview in the lower part of the dialog Right click on the preview to see the following menu Menu option Description Increase Zoom Increases or decreases the mag Decrease Zoom nification of the preview Alternatively you can hold down the Control key and move
222. ectrum then choose the Full Results Table customizable Single Soectrum template and which ever spectrum is highlighted in the Data Tree will have its results shown in this tem plate To populate a multiple spectra template hold the Ctrl key down while choosing spectra on the Data Tree and then press the Add Selected Spectra button at the bottom of the Data Tree window EDS TEM Oy 45O ND INSTRUMENTS The Business of Science Data View Current Site Data Tree Mineral Sample d Map Data 1 Spectrum 2 Fo C Spectrum 4 Do Cpp o pp Spectrum 7 Fo p d Line Data 1 Site3 Add Selected Spectra Spectra Maps Linescans To compare quant results from two spectra select Comparison of Results Two Spectra template Then select the comparison spectrum from the Compare option in the Mini Quant and Compare option The compare spectrum will be overlaid on the current spectrum in the Spectrum Viewer The quant results will be displayed in the table below Ifyou wish to change the Quant Settings press the Settings button to display the l l a Apply and Save i Quant Settings dialog Make the changes and press The recal culated results will be displayed Alternatively make the changes to the quant set Save H tings and press Press the Close button to close the Quant Settings dialog Then press the Requantify button to display the recalculated
223. ectrum 2 is the comparison spectrum You can select the comparison spectrum from a Project currently available in the Data Tree It can be from any Project any Specimen and any Site of Interest currently available in the Data tree To choose the comparison spectrum click on the down arrow Spectrum 2 in the above example Spectra available in the current Project Soecimen and Site of Interest are displayed as below Project 1 Speamenil Click on the spectrum in the display to select it for comparison The selected spectrum will be overlaid as a line spectrum over the current spectrum The MiniQuant results are displayed in a table as shown in the example below 196 EDS SEM CK HE INSTRUMENTS The Business of Science Spectrum 1 Spectrum 2 The results are displayed as wt weight The statistical error is displayed as o weight sigma for the calculated wt It is the overall confidence figure for the analysis You can use sigma to assess the results especially when an element is present at low concentration For example if an element concentration is 0 2 wt and the ais 0 12 wt the element might be detected at a statistically significant level if the acquisition time for the spectrum is extended If the is 0 4 wt it is pointless to extend the acquisition time and it is safe to assume that the element if present is at a level above the limit of detection for this technique Press to display the
224. ed drop down list l l l diodes are installed and configured FSD only FSD Z Contrast uses upper and side FSD detector channel images Select this mode if you are inter ested in seeing density atomic Z contrast signal FSD Topo Orientation uses lower FSD detector chan nel images Select this mode if you are interested in seeing orientation contrast signal Custom include and exclude FSD detector channel images of your choice When you select either of the first two modes the soft ware automatically uses the FSD diode channels asso ciated with that mode For example FSD Z mixing mode uses the upper and side FSD diode channels The FSD Topo Orientation mixing mode always uses the lower FSD diode channels Custom mode allows you to mix any FSD diode channels 126 EDS SEM The Business of Science Control Description Select Second Image Selects further images to compare with the electron images for example a forward scattered electron image This control is available only when the map dis play is for an image only a oo m Sets the number of images per row in the Standard and Interactive displays L FSD only Offers a choice of image display Standard you can add individual images or remove FSD only them from the mixed image a Interactive similar to Standard You can also change the weighting and color contributed by each image Summary similar
225. ed Enabled or Disabled None Selected Enabled Disabled Indicates file that has been used to char acterize detector Calculated File based Quant Results View The information displayed in the Quant Results View depends on which template has been selected You can view Spectrum Details Spectrum Processing and Diagnostics table in addi tion to quant results See Also Quant Settings on page 334 Element Lists on page 191 Compare Spectra amp MiniQuant Results on page 318 35 Compare Spectra Compare Spectra This step in both the Point amp ID and Analyzer Navigators allows you to compare spectra acquired from different sites of interest and specimens from the currently opened projects You can compare spectra acquired using different settings for example energy ranges 0 10 0 20 or 0 40 keV and number of channels 1024 2048 or 4096 Spectra associated with the current Site can be added to the Compare table by holding down the control key and pressing Add Selected Spectra Note that if you have acquired the spec tra in Point amp ID the positions of all the spectra associated with the current Site of Interest are displayed on the image You can add spectra from any Project Specimen and Site of Inter est from the Data tree into this table Select which spectra you wish to compare by selecting them individually from the Data Tree Press Add Selected Spectra This will add all the spectra you wish to comp
226. ed You can change the colors in the phase maps to better represent interesting groups of ele ments or phases On the Image tab top left you can view any image in your project such as the EDS layered image The Phases tab shows the combination of images that you select from the many phase maps and the electron image The spectrum bottom left shows a spectrum extracted from the pixels in the cur rently selected phase You can also closely examine the spectrum at any point or area of interest using tools on the left toolbar Phase Details bottom right shows the area of each phase in pixels and as a per centage of the total area of the map You can copy these results into a spreadsheet Toolbars around the window enable you to change the processing of the data and display and analyze the data See Also About phase maps on page 377 Analyze Phases toolbars on page 383 226 EDS SEM ON INSTRUMENTS The Business of Science Finding phases In the Analyze Phases step the software automatically converts X ray maps into phase maps The phase maps help you to see the constituent elements of the phase and how the phases are distributed over the specimen You can run this step while map data is acquired or after wards If map data is being acquired the phase analysis repeats periodically until acquisition finishes or you click the Cancel Processing button The phase analysis produces the best results if
227. ed from the spectrum by the pulse pile up procedure The pile up peaks need to be removed from the spectrum because if left they can be mis assigned as characteristic X ray lines of elements which are not present in the specimen The AIO spectrum below contains pile up peaks which are identified as P and Ag 72 gt lt 0e PD EDS SEM INSTRUMENTS The Business of Science When pile up correction is applied to a spectrum the pile up artifacts are removed but there is no indication of where in the spectrum the correction has been applied The pile up cor rected spectrum is shown below When the Show No Pile Up Correction option is checked the current spectrum is overlaid with a version that has no pile up correction applied to it The differences seen between the pile up corrected spectrum and the Show No Pile Up Correction overlay indicate where the pile up artifacts have been removed from the spectrum as shown in the spectrum below The overlay can help to identify which peaks in a spectrum are pile up peaks Al2O3 No Pulse Pile Up Comection See Also Pulse Pile Up Correction Confirm Elements Tools A toolbar is located near the top left side of the Confirm Elements step There are five dif ferent tools to manipulate the spectrum These are Pan Normalize Annotations Show Data Values and Show Candidate Elements Pan The Pan tool allows to expand the spectrum along the vertical axi
228. ed with an EBSD map the X ray data is now included with that map when reanalysed EDS data is viewed and reported together with the EBSD reanalyzed maps Extract point EBSP and X ray spectrum from any stored map data including reana lyzed data See Reanalysis on page 465 Live Monitoring This feature monitors orientation information EBSP unit cell pole figures in real time to val idate data quality During acquisition the orientation information quadrant of Construct Maps provides the fol lowing information The EBSP with optional overlay of the pattern centre and solution simulation The 3Dunit cell and list of reflectors Selected pole figure with orientation of current pixel highlighted The refresh rate is selectable up to 1 pattern per second Acquisition speed is not affected If a solution is available the name of the phase number of bands MAD and Euler angles from the collecting point also display at the bottom of the orientation information quadrant Switch between monitoring live acquired patterns and stored patterns mode via a Toolbar The live unprocessed and processed pattern are also available in Mini View See Optimize Solver on page 444 Phase fraction When collecting an EBSD map the system now gives the phase fraction of the phases found Provides a real time overview of the phases and phase fraction in the sample Avoids the need to export data to Channel 5 to see the
229. ediately Note The Quant Settings in the MiniQuant and Calculate Composition are the same Updat ing one updates the other and vice versa 183 EDS SEM ON INSTRUMENTS The Business of Science Calculate Composition amp Calculate Composition In this step you can view quant results in more detail using any of the Available Templates To view result select the template that you wish to use Available Templates Quant Result Details summary Table Single Spectrum Label Line Sum Spectrum eee aree pa gada Element List Type Current Spectrum summary Table Multiple Spectra Processing Option All Elements Full Results Table customizable Single Spectrum Coating Element Carbon spectrum Details Details Coating Thickness 15 nm Coating Density 2 25 gm Automatic Line Selection Enabled Copy Ifyou want to see a comprehensive set of results from a single spectrum then choose the Full Results Table customizable Single Soectrum template and which ever spectrum Is highlighted in the Data Tree will have its results shown in this tem plate To populate a multiple spectra template hold the Ctrl key down while choosing spectra on the Data Tree and then press the Add Selected Spectra button at the bottom of the Data Tree window 185 Data View Current Site Data Tree Mineral Sample d Map Data 1 VG Spectrum 2 GL Spectrum 4 Do Cp o TE Spectrum 7
230. eful func tion for com paring two spectra acquired using dif ferent input X ray count rates for example spectra acquired with two dif ferent beam currents Nor malize is available from the toolbar on the left of the screen in Acquire Spectra Con firm Ele ments Acquire amp Confirm and Compare Spectra steps of Point amp ID and Analyzer For details of how to nor malize using a point or a The Business of Science Context Menu Item region ona spectrum see the Com pare Spectra help topic Note that Normalize can be switched on and off from the shortcut menu avail able as right mouse click in the spec trum viewer If a point or region has already been defined on the spec trum switch ing Normalize on or off will maintain the point or region If a point or region has not been defined already switching it on will nor malize the spectra to the peak at zero EDS TEM 252 328 Context Menu Item Smooth This is useful when com paring spec tra where small dif ferences may be obscured by Statistical scatter The smooth func tion applies an energy dependent filter to the spectrum This has the effect of slightly broadening the peaks and also fil tering out the rapid fluctuations due to sta tistics Sta tistical fluctuations can some times appear like areal peak When it is difficult to decide whether a peak is
231. egories Pre defined Elements elements expected in specimen Identified Elements typically based on automatic peak identification Auto ID Fixed List used for Quantitative analysis Pre defined Elements You may have prior knowledge of your Specimen and know what elements to look for Examples I want to look for a particular list of elements I am not interested in any other ele ments may want to see their labels on spectra their X ray maps or both I want to see these even if the element is not present I know what s in my sample I want to look for a specific set of elements I want to see these even if the element is not present but I would like to know if there is anything else in my sample too You can define these elements in the Pre defined Elements tab in the Describe Specimen step If you want to save the Pre defined Elements to a profile you must first press Save to Profile button then save the profile via the drop down menu When you want to analyze your Specimen you can load this profile or another profile by pressing the Load Profile but ton in the Describe Specimen step as shown in the screen shot below 81 Spec men Geometn Pre defined Elements Press this to load a profile for your Load from Profile analysis Predefine your elements from the Periodic table Click on an element first to select it and then press the Include button Save to Pr
232. elected acquisition continues until enough counts are collected in the spec trum for quantification You can choose to terminate acquisition at the end of a preset Live Time Enter the required time in seconds into the text box This is the time for which the system is processing counts into the spectrum The live time clock runs slower than the real time clock so that the acqui sition for 100 live seconds takes longer than 100 real seconds This time is extended to com pensate for the output rate being less than the input rate by the degree of Deadtime You can choose to terminate acquisition at the end of a preset number of counts Enter the value in the Count Limit text box The default value is 500 000 Pulse Pile Up Correction Check Pulse Pileup Correction check box if you wish to automatically correct the spectrum for pulse pileup peaks Uncheck the box if you wish to disable this correction Pileup peaks can occur when a second pulse arrives and triggers the measuring system dur ing the time required to process a previous pulse When this happens neither pulse will appear in its correct position The result being a peak at a higher energy equivalent to the sum of the energy of the two photons The largest pileup peaks will be seen at twice the energy of the main peaks e g Fe Ka pile up peaks will be seen around 12 8 keV Notes The pileup correction algorithm assumes that the count rate at every energy is constant throughou
233. eloped The Position tab displays the activity Not Moving Moving In and Moving Out There are three buttons on the Position tab of the Si Li Detector Control In Out and Stop These controls are used to move the detector in and out of the chamber and stop it at the current position Shutter If the detector has a pneumatic shutter there will be a tab for the shutter control The Shutter tab has two buttons Open and Close to allow the shutter to be opened and closed The status of the shutter is either Open or Closed 488 The Business of Science EBSD Detector Control Hardware Control The EBSD detector control sets the position of the EBSD detector and displays its position and movement You can access this control from the status bar State Description States Fully Inserted Fully Retracted Intermediate Position Reference Position Auto Retracted The detector is moved as far into the chamber as the mechanical end stop allows This position is set by the service engineer and cannot be changed by the customer The detector has moved as far out of the chamber as it can The detector is at an inserted position that is not the fully inserted position or the reference posi tion The detector is at the position that has been saved as a ref erence position by use of the handset The Touch Sensor has been triggered and the detector has moved all the way out to the home
234. elp on each application follow the links below Acquire Spectra on page 313 Confirm Elements on page 330 Calculate Composition on page 355 341 Point amp ID Guided Point amp ID is an image centric application that requires the acquisition of an electron image prior to X ray spectra acquisition There are two modes of operation Guided and Custom In the Guided mode the Point amp ID navigator has six steps Describe Specimen _ 2 222 022 2 eee eee e cece cece ec cceeceeeeeeees 343 Scam Maje saaa ae a GE 346 Acquire Spectra 2 22 22 022 cece 0000000000000020 ceeeeeeeee 350 Confirm Elements 2 222 002 2 eee eee cece cece ccc cecceeeeceeeeeeeeees 353 Calculate Composition 2 2 222 22 cee eee cece eee e eee ceeeeeees 355 Compare Spectra 0000000000000000 cei eh eee hehe ab ehe nbd bes 358 342 EDS TEM Oy 45O ND INSTRUMENTS The Business of Science Describe Specimen 0 Describe specimen In this step there are two tabs Summary and Pre defined Elements Summary In the Summary view you can write notes on the Project and the Specimen present in the Project For convenience you can also copy images diagrams and text from other doc uments emails and paste into these windows Notes are saved with the Project and you are allowed to edit notes in any step of the Navigator It helps to capture the important infor mation during the analysis Cl
235. emplates if you do not select System from the Directory drop down list m Current User shows your own templates They are available only when you logon to your user account a All Users shows templates you share with other users on the same computer and possibly on the same network depending on the network configuration Using the dialog buttons The buttons around the dialog allow you to print or email the report for example Button Description Updates the list of templates here if you have added a new tem plate or changed a template design or changed some con figuration information Opens a dialog where you can generate your own report tem 47 Button Description Save As Asks for a file name then saves the selected report as a Micro soft Word or Excel file Alternatively you can double click a template in the list The default location for your new report is in the Reports sub directory of your current project Appends your selected report to the open file if a report file is already open Generates a report and prints it immediately on your default printer As an alternative you can use Save As and print the doc ument later Email Sends the report using the default email package installed on your computer Set As Sets the selected template as your preferred default report tem Default plate for the current navigator For example you can change the current template to Excel format instead of
236. en 1 4 lt gt Sitel _ Electron Image 1 Line Data 1 Line Data 2 Line Data 3 Line Sum Spectrum Mg Kal 2 Ti Kal Cr Kal Mn Kal Fe Kal Br Lol 2 The Line item is the container for EDS Data All linescans and the sum spectrum are contained within the EDS Data 34 Getting started Oy 45O ND INSTRUMENTS The Business af Science The Linescans can be processed as Windows Integral Linescans TruLines or QuantLines The Data Tree is populated with the appropriate Linescans on selection of the processing option Windows Integral Lines The standard element linescans obtained from can the counts in the element energy windows including the background TruLine The Linescans are corrected for peak overlaps and any false variations due to X ray background QuantLine The linescans are processed to show relative per centages of each element by weight or number of atoms The label of the element linescan is composed of the element symbol followed by the lines series used for TruLine Window Integral data analysis For example Cr Kal is the label for a Chromium Linescan obtained from the Kal line _ Line Sum Spectrum The sum spectrum is called Line Sum Spectrum The region the spectrum comes from is visible on the electron image This is the same region as where the linescan data is acquired from EBSD Data Folder The EBSD Data folder is the container for the six Map components
237. endi hendes d aaea Aai 273 Ddo 00 lt 1 MO 276 SCAN TAO 6 vee cenn cee seedacsuanmoneaccaaewes dacneeacs aadoasuusebeaiaconsecseoenseecsenste 280 Acquire Spectra a a 0000000000000 0000000000000 0000000000000000 a aoaaa aoaaa 284 Confirm Analysis 00 000000000000000000000 ccc ee cece cece cece cece cece eeeeeeeeeeeeeeeeeeees 287 Calculate Layers 20 222 c cece cece cece cece eee eee eee ee eee cece ence eens eeeees 292 Edit Materials s cec cccemecdne deters deamhbentaacouedueebeeoadacsusnduoedavadieeeesmeusekeears 294 Simulate SD CCE Gay unc tect ce hbo due E een deed 296 Set Up SOV Secondo enn ons bucsete dae eeunisn eet cian ane aaa son senceaes 299 LayerProbe SettingS 2 2 0 0 clo e cece cece cece eee eee eee eee ee ee eeeeeeeee sees 301 EDS EM cs 303 Optimize 2 2 cece eee ee eee eee eee eee eee eee cence cece eee aaan 305 Calibrate 2 0000 ee a nn Tea ne 306 Calibration Element 2 0 2 202 c cece ccc cece cece cece cece ec eeeceeeceeeeeeeeeees 308 Analyzer Guided 0a000000000000000000000000 000000 uaaa aiaiaaeo aoaaa araar nanan annnnn 309 Pes ribe o pecite eree rice ces E EAEE 310 Acguire Specii dpsie re a ee 313 Confirm Elements aaao aoaaa aana 2c cece aoaaa eee aaa aaa aLaaa ALLAL LaaLa aLaaa aoaaa 330 Calculate Composition 2 222 cece ee eee eee eee aoaaa 332 Compare Spectra 2222 ccc ee eee ce ee eee eee cence eens 338 Analyzer CUSTOM sek cect ee hbase eae tote eet eee beae
238. energies TruLine also known as Filtered Least Squares FLS applies further processing Sometimes the standard X ray mapping Line gives misleading results because some elements have overlapping energy windows For example a Titanium linescan 389 390 might include Barium information The TruLine option eliminates the problem by comparing the X ray line series with the expected peak shape for each element The linescans are corrected for peak overlaps and any false variations due to X ray back ground QuantLine further processes the data showing the atomic or weight percentages of elements at every point on the line EDS TEM OxKFC INSTRUMENTS The Business af Science Acquiring linescans The elements for which linescans are being acquired are chosen in the Describe Specimen step by selecting the Auto ID option Pre defined Elements or both To see the acquisition settings click the Settings cog in the toolbar in the title bar 1 Select man the Acquire Line tool from the toolbar on the left 2 Click on the image to set the start point and then drag the mouse to define the line Release the mouse to set the end point A line with start and end points is defined on the image START o a 3 Press to start acquisition A relevant section of the image is zoomed and rotated above the Linescan viewer This action aligns the defined line hor izontally to match the x axis of the Linescan viewer
239. ent Lists on page 191 Data Tree on page 85 Mini View on page 93 Step Notes on page 94 312 EDS TEM The Business af Science Acquire Spectra hs Acquire Spectra Analyzer is microscope centric application You can acquire a spectrum from a point or an area on the specimen either generated by a static probe or in STEM mode There is an acquisition toolbar near the top of the workspace It has controls for starting and stopping the spectrum acquisition There is a Settings cog for selecting the acquisition parameters For details see Acquire Spec tra Settings below The toolbar located on the left side of the workspace has various tools for spectrum manip ulation and annotation as shown in the screen shot below Tools to pan normalize add annotations and show data values Drop downs with alternative options For description of each tool see Acquire Spectra Toolbar on page 316 The Compare Spectra amp MiniQuant Results on page 318 option is available in the top right corner of the Spectrum viewer You can compare the current spectrum with any other spec trum from an opened Project on the Data Tree Instant MiniQuant results can be viewed in a table or a bar chart A number of useful shortcut menus are available as right mouse click in the spectrum viewer For details see Context Menus Spectrum Viewer on page 321 Acquire Spectra Settings The settings are described in detail below Energ
240. ent list l E oni Be Select an Element list for the Fixed List quantitative analysis from Fixed List and Current Spectrum the three options Iron Element Quant Line Fixed Weight Iron A Titanium Wy Fe and Ti are selected as the Fixed List Add element Remove element Clear all elements elements but you can overide the choice if required Element List Quant Element List Details Current Spectrum This list includes the Pre defined Elements and elements identified by Auto ID and manually using the Candidate Element tool Fixed List You select the Fixed List option if you know what elements you wish to quantify Choose the elements from the drop down list as shown in the screen shot above Fixed List and Current Spectrum To quantify the elements in the above two lists select the Fixed List and Current Spectrum option MiniQuant results table will clearly display which list is being used A lock icon will be dis played against the Fixed List elements as shown in the screen shot below 179 Sum Spectrum Compare In this example Fe and Ti are selected in the Fixed List The rest of the elements in the chart results are from the Current Spectrum because the Element List selected for quantification was Fixed List and Current Spectrum Note that the Fixed List is saved in a User Profile See also Describe Specimen on page 76 Acquire Spectra on page 350 Confirm Elements on
241. ents Note that you can normalize spectra using a point or a region Normalize Spectra Point e Select this option from the toolbar near the top left of the Compare Spectra screen e Double click in the spectrum to set a normalization point along the X axis e A window is drawn on either side of this point The spectra in the Compare viewer are scaled to the average value of cps eV Y axis in the window Normalize Spectra Region e Select this option from the toolbar near the top left of the Compare Spectra screen e Click and drag to set a normalization region along the X axis e The spectra in the Compare viewer are scaled to the average value of cps eV Y axis in the normalization region selected in the previous step Smooth The Smooth function is available from the context menus of the spectrum viewer This is use ful when comparing spectra where small differences may be obscured by statistical scatter The smooth function applies an energy dependent filter to the spectrum This has the effect of slightly broadening the peaks and also filtering out the rapid fluctuations due to statistics Statistical fluctuations can sometimes appear like a real peak When it is difficult to decide whether a peak is present or not the smooth function substantially reduces the statistical fluctuation so that any real peak becomes more visible 339 Analyzer Custom cee There are two modes of operation in the Analyzer application Guided
242. ep navigate to the Acquire Spectra step Select the Point Tool from the toolbar on the left of the window Click on different locations on the image to define multiple points Select an area selection tool from the Rectangle Ellipse and Freehand in the toolbar on the left of the window Click and drag the mouse to outline a rectangular ellipsoid or irregular shaped area on the image with the Rectangle Ellipse or Freehand Tool respectively 149 Spectrum acquisition starts in the order you have defined the points and areas Status of each point area is color coded i e current point area from which a spec trum is being acquired is yellow all queued up points areas are blue and post acqui sition points areas are white All points and areas defined on the image are labeled as Spectrum x 1 2 3 As spectra are being acquired they are added to the Data Tree just below the image they are acquired from Spectrum Acquisition Tools There is a toolbar on the left side of the Acquire Spectra and Acquire amp Confirm windows that has four point and area selection tools You can use these tools to define points and regions on an image to acquire spectra See the table below for detailed description of each tool Spectrum Acquisition Tools Point Click on this icon to select the Point Tool from the toolbar and then click on the image to start the spectrum acquisition from that point This is a useful tool for quick
243. er is created The Project folder contains a Project file with an oip Oxford Instruments Project extension By default the Project folder and Project file use the same project name however it is possible to rename either of these pro vided the project is not open in the software A Project folder may contain two sub folders data and reports Acquired data Is either stored in the oip file or in the data folder if additional data files are required It is possible for a Project to not have a data sub folder The reports folder is the default location for saving any reports generated from the Project by the user Reports can be saved in other locations where necessary Before moving a project please close any reports saved in the reports subfolder An example of a project folder is shown in the screen shot below Mew Project Name Date modified Type SIZE data 1703 2011 13 34 File folder di reports 170r 0l 13 45 File folder New Projectoip 1703 2011 13 49 OTF File 17 108 KE To move the project either copy or move the Project folder to it s new location This will main tain the folder structure and allow the project to be opened from it s new location The Project can be opened on a second PC provided the software and an appropriate license are installed To open the Project Launch the software either from the shortcut on the desktop or from the Oxford Instruments NanoAna
244. erProbe OXF INSTRUMENTS The Business of Science tems Note that if you import a model edit some of the values previous settings in the user profile can be restored by pressing Restore Layer Structure Defining the composition of each Layer Enter the composition of the substrate first followed by the individual layers The layer details shown are of the currently selected layer For each layer the composition is specified by one of the two methods either by selecting an entry from the materials database or by manually entering the com position as a chemical formula or in weight a When you select an entry from the materials database all the relevant fields for the layer composition will be automatically populated a Select the Manual entry radio button to manually enter the layer details To enter the composition choose one of the two modes of entry Number of Atoms or Weight Selecting Number of Atoms allows the entry of the chemical formula e g Al203 for aluminium oxide Selecting Weight allows entry by specifying the elements and weight values e g A 52 93047 07 Defining the density of each layer Ifyou know the density of a layer enter it in the Density text box It is expressed in g cm3 Note that when a composition containing a single element is entered the density is auto matically set to the element density Internally LayerProbe calculates the mass thickness of each layer The
245. eral different ways of exporting the linescans Save As Copy Print and Email The exported image includes the rel evant information from the Caliper or Show data values tool To export some or all of the data to a spreadsheet program such as Microsoft Excel i 2 e 4 See Also On the toolbar above the linescan viewer select Table from the drop down list To select all the data click one row in the table then press Control and A To select only some of the data click a row then drag or use click and Shift click Right click and select Copy Paste the data into your spreadsheet Toolbars on page 253 400 EDS TEM The Business af Science Extracting a single spectrum from the linescan You can examine the spectrum and element quantities at any point along the line 1 In the toolbar on the left of the image viewer click the Reconstruct Line Point Spec trum tool 2 Move the cursor to any point on a line in the linescan viewer 3 Click to extract the spectrum for the point into the project You can view the spectrum in the Mini View The data is also saved in the Data Tree with this icon 401 Extracting multiple spectra from the linescan You can examine the spectrum and element quantities at many points along the line To pre vent an excessive amount of data you can apply a binning factor to limit the number of points 1 Click the Extract Spectra button below the linescan
246. ere should not be any peaks within 100 eV of the cal ibration peak To perform Energy Calibration follow the steps Select Energy Calibration from the Calibration Routine drop down list Select an element from the Calibration Element drop down list Get the element standard in the field of view of the microscope Adjust the working distance to the recommended value and the beam current to achieve an optimum count rate 67 gt START E a Press to start acquisition of the calibration spectrum The current set tings will be used to acquire the spectrum A window will be painted across the peaks of the element X ray line series A progress bar near the top of the Calibrate window displays the estimated time for the completion of calibration spectrum acquisition On completion of spectrum acquisition a message is displayed asking you if you wish to perform the Energy Calibration Press Yes if you wish to perform the Energy Calibration Note that the details of the Energy Calibration can be found in the Spectrum Details dialog in the Calculate Composition step when a spectrum has been quantified Details on Beam Measurement For Beam Measurement you must use a pure element standard and it must be stable under the beam See Calibration Element Note that the acquisition settings chosen in the Acquire Spectra step are carried across to the Optimize Navigator and vice versa Changing the settings in one will auto
247. ersonalized report templates User interface is easy to use and intuitive Word and Excel templates can be generated at the same time Generate multiple page templates a A4 Letter format Portrait and landscape layouts See Generating your own report template on page 51 Licensing improvements AZtec and INCA Extensive improvements have been made to the AZtec INCA license activation deactivation process If a PC where you installed the software products does not have access to the inter net you need a unique unlock code from the internet based licensing service to enable you to use the software product This long code needed to be manually cop ied and taken to a PC with internet access where it had to be manually pasted There is now no need to manually copy and paste the long licence acti vation deactivation codes from one PC to another The Licence Manager automatically detects whether a USB stick is inserted in the PC and stores or loads any codes relevant to the current activation deactivation process The License Manager utility is also copied to the USB stick for use on internet PCs without AZtec software installed An extensive user guide is included in the AZtec help Note except when there is no internet access and no possibility to bring storage media to and from the system PC Network Licensing AZtec and INCA An AZtec Network licence is now available which makes AZtec INCA available to
248. ertical Scale Type a Linear shows a regular spaced grid Logarithmic is useful for dis playing data that has a wide range Show Horizontal Scale Shows the scales of keV and Show Vertical Scale cps eV Lock Vertical Scale Prevents the Pan tool from moving Lock Horizontal Scale the graph Smooth Spectrum Shows a smooth representation of the normally spiky spectrum Expand Mini Quant Shows the expanded Mini Quant display in the top right corner of the spectrum Noise Peak Shows the noise peak and includes its value if you reset the scales using the context menu option Reset Scales Include in Scaling Exclude from Scaling Shows the noise peak but excludes its value if you reset the scales using the context menu option Reset Scales Hides the noise peak Specify the energy level in the Cutoff Energy keV box Image Viewer You can control the default display of the Image Viewer To temporarily change the current display right click it and use the context menu Rescale Image Mode Changes the scale of the image For a large image select Fill Display with Image 17 Field Description Show Acquisition Areas Show Short Names Show Header Show Color Bar Show Scale Bar Show Contrast Brightness But tons Show Annotations Show Color Key Use Image Smoothing INCA Image Export Offers a choice of display for the acquisition areas Shortens the labels for the acquisi
249. ery stable electronics you may only need to calibrate the system once in several months provided the environmental temperature of the laboratory is fairly stable A few degrees change in the environmental temperature can cause a small shift in the position of peaks The Energy Calibration routine is performed for representative Process times available energy ranges and number of channels in one operation This means if you change any of these settings soon after you perform the Energy Calibration you will not need to re cal ibrate the system See details on how to perform the routine below Beam Measurement If you are an expert user and you need more than relative concentrations and require accu rate un normalized quantitative analysis results you must perform the Beam Measurement routine Any change in the microscope settings such as accelerating voltage or lens control will lead to the change in the beam current Under these circumstances you must perform the Beam Measurement routine before you do accurate quantitative analysis Note that you do not need to perform the Beam Measurement routine if you are only inter ested in a Qualitative Analysis a Normalized Quantitative Analysis See details on how to perform the routine below Details on Energy Calibration 66 EDS SEM The Business of Science Why do we need to perform Energy Cal ibration Ambient temperature changes will alter the gain of the system and
250. es the FSD diode channels asso ciated with that mode For example FSD Z mixing mode uses the upper and side FSD diode channels The FSD Topo Orientation mixing mode always uses the lower FSD diode channels Custom mode allows you to mix any FSD diode channels Select Second Image Selects further images to compare with the electron images for example a forward scattered electron image This control is available only when the map dis play is for an image only Fm sz C Sets the number of images per row in the Standard and Interactive displays FSD only Offers a choice of image display ESD onl Standard you can add individual images or remove omy them from the mixed image Interactive similar to Standard You can also change the weighting and color contributed by each image Summary similar to Interactive and in a more com pact display Er Links images You can simultaneously manipulate all the layers using the pan or zoom controls 348 EDS TEM The Business of Science Control Description Unlinks images You can manipulate individual layers using pan or zoom controls Use the mouse wheel to zoom in and out of the image Use these tools near the bottom right of the screen to adjust manual and automatic brightness contrast and color Context Menus Right click the electron image to display context menus for copying exporting and printing images See Also Scan Image Toolbar
251. escceiee 340 Acquire and Confirm 2 202 022 c eee eee ee cee eee cee ee cece eee e cece eee eeeeee ees 341 Point amp ID Guided 2 22 22 ieee cece eee cee cece eee e eee ee ceeceeeceeeees 342 Describe Specimen 22 0222 eee eee eee cece cece cece cece eeeeeeeees 343 DCO EA iets cee aera see E ae ec een enna nannies pacar nnedceseaneur enna 346 Acquire Spectra a be cates ee datnoedcewosst ne cnacbieedenestedoldeeenctecesiesnselde les 350 Confirm Elements 2 0 22 2e cece cece eee e cece cee cee eee ceeceesceeeeeseeceeseeesees 353 Calculate COMPOSItION 2 222 cece cee eee eee eee cence eee e eens 355 Compare SO OCU Ai asec cede bende cheuddawtadouecetoubesaveteeceesusecetaveecteceesees 358 Point amp ID CUSTOM 2 222 cece cee ee cece cee cee eee e eee eee eeeeeeees 360 XIX PICO UIRe and COMM es si oa cists oy nist ea oe quaein au ese eine te ahem eee adie 361 Map s G10 6 cle eee een terete ene Teme ter a ere a eae e et ene rere mere ae eee ee 362 PAV ace UH Map Bc k Sone WOR Ee Tra ETE eT Fw AR 363 COMSIPUCUIVIADS tin 5 on tsa crn Kans r Mei aitiad Monae A ck Se aeaea 370 How binning affects the quality of your data 2 2 2 2 e eee e eee ee eee eee 373 Analyze PHa ES ssctse proce tctee cb suhaneenwazetsitete suave toh eenase estes eaveetatekeumele cae 375 PVC E EE St acerca eels ttre nee ee tse ee tates Seeger eae eee 376 PUD OUT phase TAOS cacti sk it tts ctl Ses igh el Ba ea
252. ess exist which are required for a full coating cor rection to be applied for the calculation of the quantitative results The default element is car bon the defaults for thickness and density are 10 nm and 2 25 g cm respectively Note that where appropriate the default density is that of the element at room temperature and pres sure The thickness and density may then be modified if required Pre defined Elements 76 OXFORD EDS SEM ONT Sal l SL INSTRUMENTS The Business of Science If you know what elements are present in your Specimen and you only want to see peak labels or X ray maps for those elements then you can select them in the Pre defined Ele ments tab Press the Pre defined Elements tab to access the periodic table If you wish to enable the AutoID option check the Perform AutoID During Acquisition option Summary Specimen Geometry Pre defined Elements Pre defined Elements in Specimen Load from Profile Save to Profile _ Clear All Pm sm Tb Np Pu 1 Cm Bk Include Clear E Perform Auto ID During Acquisition Double click on the element symbols that you wish to include in the analysis All the included elements will be marked with the green color key in the periodic table To save the Pre Save to Profile defined Elements in the current User Profile press It means when you load the User Profile next time these elements will be included in the analysis
253. estored from the User Profile by pressing the Restore button 2793 Scan Image Scan Image In the Scan Image step you can acquire an electron image into a Site A Site is like a folder which contains images and analyses for a particular area on a Specimen For EDS if you do not want to collect an image and just want to acquire spectra you can skip this step and go straight to the Acquire Spectra step You can have any number of images in a site Just ensure that the images you want to keep are padlocked in the data tree to stop them being overwritten as shown in the screen shot below Data View a O ai Current Site Data Tree You can toggle between saving or replacing the current image with successive image acqui sition If your specimen is drifting click the Settings cog and activate AutoLock The Scan Image step has several tools for manipulating and enhancing electron images The acquisition toolbar above the electron image and other nearby controls Scan Image toolbar a vertical toolbar on the left for manipulating and annotating the image a Ifa forward scatter electron detector FSD is fitted extra controls are available for combining the signals from each diode into a mixed image Acquisition toolbar and other nearby controls The acquisition toolbar above the electron image and below the Navigator has buttons for starting and stopping the image acquisition the Sett
254. f you know it For a pure element the density is set auto matically and is set to 1 0 for a compound 4 Press the Add button to save this material entry to the Database Name Materials are stored under unique names specified by you Each material contains one or more elements along with their atomic and weight stored with each element Composition The composition is specified as a chemical formula for example Aluminum Oxide is entered as AI203 or elements with weight AI52 926 047 074 Edit Materials Barme Aihame Chocks Ohocae yaa mp hpi hemn the opha below and then ipay a chomecal formula cg Mall fetal wmght A houd be 101 Number of fiboms Hegh Componition APO emet Joe S Wesght A 40 000 525 0 Sooo af Ora Density gom k Alem Choke 294 LayerProbe Oy 45O ND INSTRUMENTS The Business of Science When entering compositions as weight it is important to note that the total weight for a material must add up to 100 0 1 In addition you are only allowed to add valid materials valid element symbols chemical for mulae to the database A flashing red rectangle means that the material entry is not valid Density If you know the density you can enter the value of the material in g cm When a composition containing a single element is entered the density is automatically set to the element density However if a compound is entered the density is always set to 1
255. formed your EDS data is also carried into your reanalyzed map data folder This functionality is yet another pow erful tool to ensure successful phase identification and mapping In addition it allows you to extract both EBSP and EDS data point information for phase ID Setting up for Data Reanalysis In order to do any kind of reanalysis you need to be working with an EBSD Map that has stored patterns with it Either highlight a previously acquired Map with stored Patterns or create anew Map To acquire a new Map with Stored Patterns Create and save an Aztec Project Go to the Acquire Map Data step and create a Map Under Settings ensure that you tick the Store Patterns option Without the stored patterns option enabled reanalysis will not be possible Go to the Data Tree tab and confirm that under Map Data EBSD Data folder the Processed Patterns Alert Mesias is visible Optimize Acquisition settings Go to Phases tab add and or remove phases Select the phase database of your choice and add phase for acquisition In the phases for acquisition quadrant select the desired number of reflectors for each phase listed Use the Phase ID navigator step to identify any unknown phases and or confirm composition using existing EDS and EBSD data Search the phase databases for all phases using the composition ranges of the listed ele ments Go to the Acquire Data step and locate EBSP of interest to collect
256. gators allows you to compare spectra acquired from different sites of interest and specimens from the currently opened projects You can compare spectra acquired using different settings for example energy ranges 0 10 0 20 or 0 40 keV and number of channels 1024 2048 or 4096 Spectra associated with the current Site can be added to the Compare table by holding down the control key and pressing Add Selected Spectra Note that if you have acquired the spec tra in Point amp ID the positions of all the spectra associated with the current Site of Interest are displayed on the image You can add spectra from any Project Specimen and Site of Inter est from the Data tree into this table Select which spectra you wish to compare by selecting them individually from the Data Tree Press Add Selected Spectra This will add all the spectra you wish to compare into the Com pare table spectrum Label Spectrum Color Line Thickness Project Path spectrum 1 r Normal Project 1 Specimen 1 Site 1 spectrum 2 2 Normal Project 1 Specimen 1 Srte 1 spectrum 3 Normal Project 1 Specimen 1 Srte 1 If you want to remove any spectra from the table highlight the spectrum and press Remove Spectrum You can choose which of the available spectra you wish all the others to be compared to by selecting your reference spectrum from the compare table and pressing Select Reference Spectrum Settings You can change the color
257. ge is near 1 keV the low energy peaks for some ele ments might be excluded from scaling To exclude the noise peak when resetting the scales in any spectrum 1 On the Tools menu select Preferences 2 On the Preferences dialog select the EDS Spectrum Viewer tab 3 On the tab under Noise Peak select Exclude from Scaling To include the noise peak follow the same steps and instead select Include in Scaling This automatic scaling occurs whenever a new spectrum is acquired unless the vertical scale is locked To exclude the noise peak when resetting the scales in the current spectrum 1 Right click in the Spectrum Viewer to open the context menu 2 Select Noise Peak then Exclude From Scaling 3 Right click in the Spectrum Viewer to open the context menu Select Reset Scales Setting the cut off voltage for the noise peak To set the cut off voltage for the noise peak in any spectrum 1 On the Tools menu select Preferences 2 On the Preferences dialog select the EDS Spectrum Viewer tab 3 On the tab under Noise Peak select Hide or Exclude from Scaling 102 ON INSTRUMENTS The Business of Science EDS SEM 4 In the Cutoff Energy keV box type a value between 0 and 1 The recommended value is 0 12 keV If the value for cut off is near 1 keV the low energy peaks for some elements might not be vis ible or they might be excluded from scaling Context Menus Spectrum Viewer A number of usef
258. ge the default report template by selecting it from the Report Preferences or accessing the Report Templates from the down arrow on the Report Results button Managing your reports You can click the down arrow on the Report Results button to open a menu of options that enable you to manage your reports Some options are available only if Microsoft Word or Excel is installed In some cases the appearance of the Report Results button changes to indi cate the last action that you performed so for example you can send reports by email in quick succession The following menu options affect individual reports Appearance of the Description Report Results icon Information Shows the name of the report template at the top of that is selected by default for the cur the menu rent navigator AAAA AAAAA A AAAAA If no name is shown select Report Tem plates choose from a template from the list and click Set As Default Save As Asks for a file name then saves the report as a Microsoft Word or Excel file The default location for your new report is in the Reports sub directory of your current project 44 Fe Getting started INSTRUMENTS The Business of Science Appearance of the Description Report Results icon Append Appends your report to the open file if C a report is already open soft Word Asks for a file name if no report is open or Excel is installed Print Generates a report a
259. ges panel and click the required image A new EBSD image appears under the EBSD Data node in the Data Tree 464 INSTRUMENTS OARD EBSD The Business of Science 2 To display any image in the image viewer area click on the smaller image on the Data Tree Deleting EBSD Images To delete a map from the analysis completely On the Data tree or Current site right click the image and in the context menu select Delete Reanalyzing a Map region If you have acquired an EBSD map with stored EBSPs you can also to reanalyze a map region with new settings such as new solver settings or even solving by including different phases The reanalyze toolbar allows you to reanalyze a region of the complete map or entire map by selecting a rectangular elliptical or free hand region Select your desired shape region to reanalyze your EBSD map Click Start to start reanalysis Please take note that your total Area number of pixels will be dependent on the selected region Viewing Orientation information It may be helpful to view the orientation information from a point To view how the indexing has changed with different acquisition settings you can click to show orientation infor mation from point in map icon gt fromthe map area Click on the electron image and place the crosshair on the pixel desired Orientation information such as EBSP unit cell and pole figures can now be monitored The orientation informati
260. give you a single workspace called Acquire and Con struct It provides the convenience of working in one screen without having to move away from it The user interface components are docked in the four quadrants in the workspace Each com ponent can be undocked as a free floating window It can be dragged on to another monitor resized or displayed in the full screen view There is a toolbar located near the top right corner of the workspace with icons which allows you to toggle on off each component The user interface elements are described below Acquiring an electron image and line data In the top left quadrant you can acquire an electron image first and then define a line to acquire the line data E E gt START 1 Press to select the image acquisition mode Then press to start electron image acquisition 2 On completion of image acquisition press to switch to the line data acqui sition mode 3 Press aS to select the line tool in the toolbar on the left 4 Click on the image to set the start point and then drag the mouse to define the line Release the mouse to set the end point A line with start and end points is defined on the image START 5 Press to start the line data acquisition A relevant section of the image is Zoomed and rotated above the Linescan viewer This action aligns the defined line horizontally to match the x axis of the Linescan viewer Element linescans start to populate in th
261. gma confidence level for a normal statistical error distribution The Confidence Factor is used to determine how AutoID behaves with regard to the sources of error AutoID is designed to find a good combination of peak profiles that matches the spectrum and thus identifies the elements present in the specimen When peaks overlap the oe proportion of constituent profiles is determined by least squares fitting to the sum of peak profiles Counting statistics introduce fluctuations into the spectrum that are sometimes dif ficult to distinguish from genuine peaks The statistical fluctuations introduce random errors that are equally likely to be positive or negative When there are severe peak overlaps it is even more difficult to distinguish genuine peaks from noise fluctuations In addition chemical bonding effects and inaccuracies in peak profiles may mean that there is no combination of peak profiles that is an exact match to the spectrum even when there is no statistical noise If the peak profile is not perfect this introduces bias or systematic error into the results If a fitted peak profile is much larger than the random or systematic errors it is likely that the corresponding element is present in the specimen Note To access the AutoID Confidence Factor select User Profile from the Tools menu and then select the Element Settings tab AutoID Confidence Factor is available in the AutoID Settings 26 Getting started
262. good forescatter orientation contrast OC images but not always Change samples Some materials give better orientation contrast signals than others FSD images with strong orientation contrast will yield high quality EBSPs for EBSD analyses To optimize your FSD and get the best possible images you need to consider sample preparation a SEM settings sample to detector geometry Sample preparation The quality of your FSD images is highly dependent on the preparation of the sample s sur face The forescatter signal is not very strong and is easily dominated by topography rough ness Therefore sample preparation is critical For the best forescatter images the specimen must be completely flat and featureless Mechanical polishing with colloidal silica is recommended to remove relief in the sample It is an easier and similar polishing process across most materials making it ideal for polyphase samples and harder particles in a softer matrix With care a quick electropolish gives the best surface finish without introducing too much topography However electropolishing can produce rough surfaces and highlight grain boundaries Any surface topography or dirt particle is exaggerated casting shadows on the surface affecting the FSD image quality For example 427 SE image of a Mg alloy with dirt particles on FSD image of the same area showing the the surface effect of the dirt particles Coating the sample
263. gy Calibration routine is performed for representative Process times available energy ranges and number of channels in one operation This means if you change any of these settings soon after you perform the Energy Calibration you will not need to re cal ibrate the system See details on how to perform the routine below Why do we need to perform Energy Cal ibration Ambient temperature changes will alter the gain of the system and this will affect where peaks appear in the spectrum The exact peak positions and the resolution of the system are needed to precisely identify individual peak components in the Spectrum If peaks overlap the relative sizes of individual peaks can only be calculated accu rately if the width and position of each peak is accurately known By measuring the position of one known peak the system can be optimized to determine the position of all other peaks How often should I perform Energy Cal ibration The electronics used is carefully designed to provide good temperature stability Since a change of 10 C produces only a 1 eV shift in peak position most routine analysis can be per formed without re optimizing peak position However if you need the software to resolve very closely overlapped peaks you should perform Energy Calibration and re optimize if the 306 EDS TEM The Business of Science ambient temperature changes by a few degrees With a good laboratory temperature control you
264. he Livetime The calculated count rate for the simulated spectrum is not editable However it is useful to see how the calculated count rate changes when the Beam current factor or Accelerating Voltage is changed Number of Channels The numbers of channels for the simulated spectrum are user selectable 1024 2048 and 4096 Energy Range keV The energy range of the simulated spectrum used or selected is user Selectable from 0 10 0 20 and 0 40 keV The energy range to use will depend on the elements present in the specimen and the X ray lines to use for analysis Accelerating Voltage kV The accelerating voltage of a simulated spectrum is user selectable in the range from 2 0 to 30 0 kV On selection of a template spectrum in the data tree the accelerating voltage for simulation is initially set to match that of the template spectrum LayerProbe Oy 45O ND INSTRUMENTS The Business of Science Set Up Solver The purpose of this step is to investigate if a particular problem is soluble and to suggest experimental and analysis conditions to use when calculating unknown layer thicknesses and or concentrations There are various parts to this step all of which are necessary to com plete before you can calculate the Solubility 1 Make sure that the model of the structure you wish to characterize is set up cor rectly see the Describe Model step for details 2 Select a spectrum from the data tree to use as a templat
265. he full quantitative data for each point Wt or At Points can be binned by 2 4 8 16 and 32 Spectra can be extracted from any point on the linescan for further investigation This functionality is also available for Line and TruLine See Acquiring linescans on page 391 AutoPhaseMap for SEM and TEM What s New in AZtec 2 1 The Business of Science AutoPhaseMap is a new way to automatically create a map of the distribution of phases in a sample automatically during or after acquisition Turns X ray map data into Phase Map data in seconds Calculates and displays Distribution of each phase Spectrum and composition for each phase Area fraction for each phase Finds phases and highlights elements that are present at only trace amounts a Finds phases at all size ranges including nano materials See Analyze Phases on page 375 EBSD Reanalysis improvements a Live Monitoring Phase fraction Improvements in image acquisition for forescatter detectors Drift correction using FSD images as references Export Raw Unprocessed EBSPs for cross correlation application General performance and other EBSD improvements Reanalysis improvements The reanalysis functionality is now more versatile Multiple reanalysis of any map so settings can be repeatedly optimised if required This includes changing the solver settings and adding or removing phases IfSmartMap EDS data is collect
266. he relative errors are less than 2 you should standardize If you are quantifying elements whose X ray lines are in the low energy region of the spectrum which may be the case if you are using an accelerating voltage of less than 15kV or the element you are quantifying has an atomic number less than 11 standardization will improve your quantitative results If the matrix corrections are high such as would be in the case of quantifying Al in a Pd matrix e g light in heavy heavy in light where your intensity cor rection Ic is either gt 1 25 or lt 0 8 you should standardize The intensity cor rection is given in the quantitative results Not necessary to standardize if 264 EDS SEM Oy 45O ND INSTRUMENTS The Business af Science You only want to know which phase it is Your standards are of a poor quality rough dirty Getting Started with Standardization Quantitative analysis can be performed without the need to measure standard materials since your system is supplied with a complete set of Factory standardizations However in specific cases using your own standards will lead to an improvement in your quantitative results The purpose of Standardize is therefore to enable you to set up your own standards for quantitative analysis When you use your system for the first time and click on the Standardize step your own standards database will be created At this stage your database will
267. he sample image as appears in the main user interface is shown overlaid on this 1355 If the sample image reaches the edge of the dark surround that indicates the limit of Auto Lock has been reached If drift continues in that manner some parts of the sample will be out side the viewable area of the microscope Note that the software will terminate the current experiment if the tracking area or the scan region in In field mode reaches the edge Any queued experiments will be immediately canceled if they are also outside the edge of the image The trail may extend outside the sample image but not outside the total imaging area The trail will reset for each acquisition i e it will only show the drift from the current acquisition AutoLock History The AutoLock performance histogram like the drift profile trail also shows the amount of drift that has been applied during a single acquisition e g map acquisition However it pro vides a histogram view that allows rapid assessment of drift Consider the diagram below showing the histogram display Mini View AutoLock History Y Number of Measurements 16 100 lt o g 5 ae 25 Ta mill 0 5 10 Correction pixels 15 The horizontal axis shows the amount of correction applied in image pixels and the vertical axis shows the percentage of the correction that had to be applied For a stable sample the amount of correction should be low this will appear
268. he two modes of mapping during acquisition by pressing the Map or TruMap button above the map display Select the acquisition parameters from the Settings cog on the acquisition toolbar gt START and press to acquire map data from the full frame TO acquire maps froma region select a map acquisition tool from Rectangle Ellipse and Freehand tools available from the toolbar 363 364 Tools to pan normalize and add annotations Drop downs with alternative options Tools to specify rectangular elliptical and freehand regions on an electron image for map acquisition Tools to specify points and regions on an image for spectrum reconstruction Tool to show data values on an image or spectrum Click on the image and drag with the left mouse to outline a region on the image Maps will be acquired from the scanned region During TruMap acquisition a pro gressing green line is the map acquisition line followed by a yellow map processing line A layered image element maps and an electron image s SE BSE are displayed You can choose how you wish to view your data from Standard Interactive or Summary view available from the drop down list Adjust the slider bar to choose the number of maps per row The layered image allows you to see the X ray maps overlaid on the electron image You can add or remove an X ray map from the layered Image combined Electron and X ray map image by toggling the Laye
269. hich setting works best for your specimens Exposure Time Once you have selected the level of binning enter a camera exposure time also known as the integration time Even with low signal strength values the software copes very well with such EBSPs If the exposure time is set too low there will be insufficient signal in the image and it will appear too dark If the exposure time is set too high part of the image may be over sat urated forming a white area The exposure time for a given binning level will depend on the probe current you have used to collect your electron image With some microstructures it will be necessary to work with low probe currents to achieve the spatial resolution necessary to resolve the desired fea tures In this case you will need to adjust the exposure time and binning accordingly Histogram of the Unprocessed EBSP This histogram allows you to look at the distribution of pixel intensity in the unprocessed EBSP You may use the mouse wheel to adjust the size of the histogram e Signal Strength The signal strength Is a value which lies between 0 100 It corresponds to the position of where the end tail of the histogram lies on the x axis of the histogram We recommend that you use a value between 85 and 95 If the signal strength is too low or too high it will appear 437 in the red region If the signal strength is an acceptable value it will appear in the green region Anything above 9
270. his action will close the dialog and remove the backup copy Press backup copy to close the dialog This action will restore the current settings from the There are separate tabs for different settings in the User Profile dialog The details of the set tings in each tab are described in the topics which can be accessed from the links below See Also Scan Image Settings on page 421 Acquire Line Data Settings on page 252 Acquire Map Data Settings on page 211 Acquire Spectra Settings on page 313 Element Settings below Peak Labels on page 158 Quant Settings on page 187 LayerProbe Settings on page 301 EDS Element Settings The Element Settings tab in the User Profile dialog is provided with a periodic table It enables you to define a list of Pre defined Elements present in the specimen and the elements you wish to exclude from the AutoID routine When you press an element symbol in the periodic table three buttons are enabled which are colored coded Include Exclude 24 Getting started The Business of Science Clear Defining an element from the periodic table is a cyclical process Double clicking on an ele ment symbol will include this element It will be colored green Double clicking it again will exclude this from the list and it will be colored red Double clicking on the symbol third time will clear this element from the list Tip For multiple element selection hold down the Ctrl key
271. his option if you wish to define a list of elements with which to quantify your spectra For example you may only wish to quantify your spectra using certain elements if you are con stantly quantifying similar spectra Define your Fixed List using the Periodic Table To include an element in the list click on the element symbol on the Periodic Table and press Include or double click on the element symbol e Fixed List and Current Spectrum Select this option when you know what elements there are in your specimen and you also wish to include any other element that may be present You define your Fixed List using the Periodic Table as described in bullet number 2 above The Confirmed Elements List is from the Current Spectrum This list includes all the elements identified by AutoID and any other ele ments that may have been added to the Confirmed Element list manually What elements are quantified when you select Fixed List and Current Spectrum are shown in the examples below in a table 335 Fixed List Current Spectrum Combined List Spectrum 1 Si O Si O Al Ca Si O Al Ca Spectrum 2 Si O B N Si O B N Quant Element List Details From this tab you can view the details of each element in the list The default setting is that the X ray lines to be used for Quant are automatically selected You can manually select the X ray line for each element if you un check the Automatic selection of line for all elements op
272. ically possible From the same phase and orientation From the center of the field of view Under the same operating conditions such as acceleration voltage kV insertion distance ID and binning The correction factor that you acquire here is applicable only for the current conditions of working distance WD kV and ID and only during the current session We recommend that you collect this data from a silicon single crystal specimen if possible Keep the specimen at the same position or same grain if it is a polycrystalline material if at all possible to keep the same geometry conditions If a single crystal is used there is then there fore no reason to move it On the SEM set the mode with the field mode on Degauss the SEM Without moving the specimen focus the image a ee IN In the Distorted EBSP area click SNAP to snap the EBSP Information about kV WD and ID appears in the status bar below the EBSP 440 EBSD Oy 45O ND INSTRUMENTS The Business af Science 5 Click Save As and save the oimfc file to a suitable location This saves the distorted EBSP into the oimfc file 6 On the SEM set the field free mode on 7 Without moving the specimen refocus the image 8 In the Undistorted EBSP area click SNAP to snap the EBSP Information about kV WD and ID appears in the status bar below the EBSP Note that the reported WD in the field free mode might be different compared to the W
273. ick with the right mouse button on the Project or Specimen in the Data Tree and then select Edit Notes to write modify the relevant notes You can add new Specimens to the current Project by pressing the New Specimen button New Specimen Specimen 1 Click on the Specimen in the Project Overview dialog This action displays the Specimen Notes for Specimen 1 text box Here you are provided with the text formatting tools You are allowed to write notes about each Specimen and save them Pre defined Elements If you know what elements are present in your Specimen and you only want to see peak labels or X ray maps for those elements then you can select them in the Pre defined Ele ments tab Press the Pre defined Elements tab to access the periodic table If you wish to enable the AutoID option check the Perform AutoID During Acquisition option 343 Summary Specimen Geometry Pre defined Elements Pre defined Elements in Specimen Load from Profi le Save to Profile Clear All Pm 5m Eu Np Pu Am Include l Perform Auto ID Dunng Acquisition Double click on the element symbols that you wish to include in the analysis All the included elements will be marked with the green color key in the periodic table To save the Pre s Save to Profile defined Elements in the current User Profile press It means when you load the User Profile next time these elements
274. id onto the experimental spectrum The choice of peaks in the fitted spectrum is based on the elements defined for the composition of the model in the Describe Model step and their heights are obtained by individual fitting If any elements are missed the fitted spectrum will not overlay correctly on the experimental spectrum This is a useful way to confirm that the elements in the experimental spectrum are the same as defined in the model Analysis Lines 28 7 The X ray lines used for analysis Analysis Lines are displayed in the Analysis Lines table below the Spectrum Viewer Lines can be selected or deselected by checking or unchecking the relevant box Alternatively you may have used the Calculate Solubility procedure in the Set Up Solver step to optimize the analysis conditions and determine the appropriate analysis lines to use for a particular model To use these lines press the Use Selected Conditions button Quantify When Quantify is pressed the current spectrum is processed The element list is fixed and determined by the set up of the model and the deconvolution element list For each element line the peak area from FLS processing is used to calculate a k ratio which is the ratio of inten sity of the line to the intensity that would be observed froma pure element under the same conditions The intensity for the pure element is calculated from the Beam current meas urement and
275. ience Linescan Guided In the Guided mode the Linescan navigator has four steps Describe Specimen Scan Image Acquire Line Data and Construct Linescans The two new steps are described here Acquiring linescans 0 222 222 eee eee cece cece ee cece eee eeeee 391 Displaying and manipulating linescans 22 393 Measuring the distance between two points 395 Viewing element counts and percentages 2 2 396 Comparing element quantities 222 2022 22222 eee eee 397 Smoothing the linescans 222 022 c eee e eee eee e ee eee ee 398 Linescan Data 2 2 22 2 222 c occ ccc cece eee ee eee eeeee 399 Exporting the linescan data 022 0 0222 c eee cece eee eee ee 400 Extracting a single spectrum from the linescan 401 Extracting multiple spectra from the linescan 402 Construct Linescans 22 0222 2 22 ccc cece eee cece eee eee eee 403 Acquire Line Data e a i Acquire Line Data In this step you can acquire element linescans along a line defined on the electron image or map The data can be processed in several ways a Line also known as Window Integral obtains the counts in the element energy win dows including the background Line gives a fast and simple representation of the X ray
276. iewing the X ray acqui sition parameters Input Count Rate cps Output Count Rate cps Dead Time Ratemeter also displays the current Process Time and the Recommended WD mm Step Notes Step Notes provide the first time user of a navigator with simple instructions on how to com plete a typical work flow It also provides a site administrator or user with the ability to write an SOP Standard operating procedure A default editable set of notes are provided for each navigator step The user can then over write these or add notes as required A reset to default settings is available The notes are saved with the current user profile See Also Step Notes Editor on the facing page 42 Getting started Oy 45O ND INSTRUMENTS The Business of Science Step Notes Editor The editor allows you to format text as you would using a word processor You can cut paste and copy text left right and central align the text change the font size and style undo and redo select bulleted list or numbered list and paste in a picture 43 Report Results You can quickly and easily generate reports from the data in your project Each navigator has a default report template A report is generated from this template when you click the Report Results button on the main navigation bar Once the report is generated the software automatically displays the new report so you can view edit or print it You can chan
277. ificant errors if no such cor rections were applied Sample step input of additional parameters coating density and thickness Standardization here the normalized area of the standard I std I optimization is corrected for the coating Full calculations the quantitative results are corrected for the coating Described below are the expected modes of operation for the locations described above Describe Specimen step In the Describe Specimen step two parameters exist which are required for a full coating cor rection to be applied coating density and thickness This part of the program behaves in the fol lowing way 79 New project specimen For example select coating correction the default element is carbon the defaults for thickness and density are 10 nm and 2 25 g cm3 respectively Note that where appropriate the default density is that of the element at room tem perature and pressure The thickness and density may then be modified if required Existing specimen If a coating element was selected this will remain as before with the density set to the default value and the thickness set to zero With these settings the coating element will be deconvolved as before but no coating correction will take place The full coating correction will be enabled by setting the thickness to a non zero value Standardization The value of the Standard Correction Factor is adjusted to take account of the selected
278. igators that take you through your analysis from the Specimen through to the Report You can navigate backwards and forwards as you wish Each step has associated F1 context sensitive help and Step Notes to assist you at each stage of your analysis Custom Mode In this mode the key components are provided in one window It allows you to perform the analysis in one workspace without having to move away from it Each component can be undocked to have it free floating or dragged to another monitor to view it in full screen To provide you with more workspace the Navigator area can be collapsed by pressing La in the top right of the application window Press to restore the Navigator Below are some key user interface elements which make the software unique NEAL EIo e 5 Menu Bar aaan a ene eee 6 Preferences 0 000000000 000000000000 0000000000000000 0000000202222222 13 SLT aoa ee i ee eet eee 20 User ae oa 62 cae ne ee nnn ea OT ere ee 22 Support Panel 2 2 22 e ee eee 27 Report Results 2 222 222 o cece ccc e eee ce eect eceeeeceeeees 44 Themes 12 02 eee cee eee cee ee eee eee ee cece eee eeeeeeeee 53 Search Tool 22 000 2 occ c eee 00000000000000 000000000000 eee eee ee eee 54 Color key hts a a ee en th el een 55 The Business af Science Navigators Getting started The software has Navigators to guide the user through the analysis process There are the fol lowi
279. ight click and in the context menu select Merge into 3 Select the other phase from the list The first phase disappears The spectrum phase name and color of the second phase are updated to include information from the first phase See Also Analyze Phases settings on page 381 Grouping Level Phase maps in the Data Tree The EDS Data folder contains phase map data in a folder which by default is labeled as Phase Image where is an automatically increasing number For example 2220 1 Ti 2 AIMgO i 2 AIMgO 3 FeMntr ar The EDS Data container contains the Phase Image folder which contains all the phase maps L The name of a phase map is composed of a number and its elements for example 2 AlMgO To rename the phase right click the icon and select Rename A spectrum extracted from one of the phases For details right click the icon See Also Data Tree on page 85 Analyze Phases on page 375 Analyze Phases settings The software processes data acquired from the maps according to the settings for Boundary Threshold and Grouping Level To see the settings click on the Settings button The default settings are stored in the User Profile Find Phases Ph Settings AutoPhaseMap Settings settings Mode Default Custom Boundary Tolerance 3 0 Grouping Level 2 0 Boundary Tolerance Boundary tolerance controls the behavior at the boundaries of each phase 230
280. ight to the Acquire Spectra step You can have any number of images in a site Just ensure that the images you want to keep are padlocked in the data tree to stop them being overwritten as shown in the screen shot below Data View Current Site Data Tree a O You can toggle between saving or replacing the current image with successive image acqui sition If your specimen is drifting click the Settings cog and activate AutoLock The Scan Image step has several tools for manipulating and enhancing electron images The acquisition toolbar above the electron image and other nearby controls Scan Image toolbar a vertical toolbar on the left for manipulating and annotating the image a Ifa forward scatter electron detector FSD is fitted extra controls are available for combining the signals from each diode into a mixed image Acquisition toolbar and other nearby controls The acquisition toolbar above the electron image and below the Navigator has buttons for starting and stopping the image acquisition the Settings cog for selecting the image acqui sition parameters and a button to link unlink images for manipulation F New Site Scan Image E START STOP Settings Select Second Image None 3 346 The Business of Science Control FSD only EDS TEM Description Displays up to three combinations of mixed image and individual images Your selections are retained in your
281. image Acquisition will immediately start under conditions currently set for both EDS and EBSD EBSD acquisition will use the settings currently set in Optimize Pattern EDS acquisition will use the parameters currently set under EDS Settings Please select the link below for details on EDS Acquisition settings A Point Data node will immediately appear both in the Data Tree and Current Site views The associated collected data EDS Spectrum and EBSP will be grouped together under this node with a corresponding label Note that this label can be renamed by selecting the rename option from the context menu on the Data tree and Current Site Data Views Depending on the acquisition settings EDS and EBSD could be acquiring for different lengths however acquisition will continue until both spectrum and pattern acquisition are complete The progress of acquisition is displayed on the Current Site tab on the Point Data node You may queue up several points to acquire data from by clicking with the acquisition tool on the electron image Acquisition will continue until all the data has been acquired or the stop button is pressed Note that the corresponding points are marked on the electron image See Also Acquire Data EDS Settings Context Menus Image Viewer on page 157 Context Menus Spectrum Viewer on page 321 Compare Spectra amp MiniQuant Results on page 195 Current Site on page 29 Data Tree on page 85 476 EBSD Oy 45O ND
282. ines can In this case you should use a shorter Process Time which will mean that you can work with higher acquisition rates and shorter acquisition times The choice of Proc ess Time will very much depend on your sample and what you wish to do with your SmartMap data once it has been acquired 3 If you have started your Project in Map and you are analyzing an unknown sample we recommend that you use a long Process Time in order that you do not miss any detail in your spectrum However if you only wish to map certain elements whose 315 main lines do not overlap you can afford to shorten the Process Time and increase the acquisition rate by increasing the beam current Acquisition Mode There are three options to terminate the acquisition Auto Live Time and Counts If Auto mode is selected acquisition continues until enough counts are collected in the spec trum for quantification You can choose to terminate acquisition at the end of a preset Live Time Enter the required time in seconds into the text box This is the time for which the system is processing counts into the spectrum The live time clock runs slower than the real time clock so that the acqui sition for 100 live seconds takes longer than 100 real seconds This time is extended to com pensate for the output rate being less than the input rate by the degree of Deadtime You can choose to terminate acquisition at the end of a preset number of counts Enter the v
283. iness af Science EBSD Data Folder The EBSD Data folder is the container for the six Map components as shown in the screen shot below Map Data 1 a PEJ EBSD Data P Band Contrast 1 bap Phase Color 1 a Euler Color 1 IPF IPF X Color 1 IPF Y Color 1 IPF Z Color 1 EBSD Layered Image 1 IPF IPF These components are described briefly with their respective icons Band Contrast Band Contrast is an EBSP quality number higher the number more contrast there is in the EBSP Phase Color This component colors the pixels in the map based on which phase was identified The color for each phase is defined in Phases for Acquisition Iot Euler Color The Map component colors the map based on the Euler color scheme and will help to show different orientations within the map Euler 1 R Euler 2 G Euler 3 B 91 IPF IPF X Color IPF Y Color IPF Z Color The IPF color components color the pixels based on the orientation of the unit cell and chosen reference direction x y or z Note that the color key depends on the structure type so it is not always the easiest map to interpret EBSD Layered Image A Layered Image is a composite image created from electron and EBSD map images or ele ment maps if EDS is present as shown in the screenshot above Point Data In Phase ID a Point Data node appears in the Data tree when spectra and EBSP are acquired from the points defined o
284. ing a Oxford Instruments Website This opens the Oxford Instruments Website Support 61 62 This links to Oxford Instruments Support Website a NanoAnalysis Encyclopedia This opens the Encyclopedia that contains help topics with interactive diagrams and movies It provides the background information theory and instrumentation of Microanalysis techniques e Show Nano Analysis Advice It has a number of topics which provide step by step advice on most frequently performed tasks e Launch User Manual This opens the User Manual in PDF format The manual is supplied with a table of content and a comprehensive Index e Launch Nano Analysis Encyclopedia This is another way of launching the Encyclopedia E Visit Oxford Instruments Website This launches Oxford Instruments website e About The About dialog opens It has Software version number and Copyright statement You can access License information System information Assembly information and Credits e Search Help The Search Help field is near the top right corner of the application window To find a single word or any combination of words type each keyword here To find a specific phrase include double quote marks around the keywords Then press The Help Viewer is displayed with links to a list of topics containing the keywords or the phrase When you click a topic link the topic is displayed in the Help Viewer You can go back through
285. ing EBSD data pause resume and restart icons are also shown Progress infor mation is also shown in the tool tip Pending Acquisitions Spectrum shows a cancel icon Spectrum 3 Note spectra and map acquisitions can be queued See Also Data Tree on page 85 Data Tree Menus on page 38 29 Data Tree Data is archived in a logical manner and can be directly viewed via easily recognizable icons on the Data Tree To access the Data Tree select the Data Tree tab on the Data View panel All open Projects and their contents are displayed in the Data Tree Multiple Projects can be opened and shown in the Data Tree at the same time If you have multiple Projects Spec imens or Multiple Sites in the Data Tree you can easily get to your current site by pressing the Current Site tab When the application is started a default Project containing a Specimen and a Site is shown As you acquire data items are added to the Data Tree The current items in the Data Tree are shown in bold Click on an item on the Data Tree to make it current Items on the Data Tree The screen shot below shows an example of the main items in the Data Tree Each item is described along with their icons below Data View Current Site Data Tree Project 1 i Specimen 1 4 C Sitel _ Electron Image 1 spectrum 1 Spectrum 2 mo Project Project is a top level container for data Each Project is associated with a folder on the file s
286. ing from spurious peaks To exclude any element from the quantitative calculation select the required element s from the drop down list and press Add element More than one element can be selected for deconvolution To remove any elements from the list high light the required element and press Remove element The peaks associated with all the elements which have been selected for deconvolution will automatically be decon volved from the spectrum prior to quantification This procedure involves fitting to the peak and removing the peak s contribution from the spectrum This becomes impor tant when there is an overlap with neighbouring peaks Thresholding 289 If thresholding is enabled any X ray line whose k ratio value is below the minimum value allowed by the Stratagem engine is assigned the minimum allowed k ratio value in order for the calculation to proceed without an error message a Window artefacts If you check the Correct for Window artefacts box a correction is applied to com pensate for the presence of a thin window in front of the X ray detector In some situations you may observe a carbon K energy peak in the spectrum even though there is no carbon in your specimen This is an artefact caused by the detector vacuum window The real background bremsstrahlung spectrum should be smooth with no bump at Carbon The thin detector window is made from polymer with a high carbon content and the absorption
287. ings cog for selecting the image acqui sition parameters and a button to link unlink images for manipulation F New Site Scan Image E START STOP Settings Select Second Image None 3 g g g 280 The Business of Science Control FSD only LayerProbe Description Displays up to three combinations of mixed image and individual images Your selections are retained in your user profile Click to start the image acquisition according to the cur rent acquisition parameters Click to stop image acquisition Acquisition stops at the end of the current frame Click again to stop imme diately If you navigate away from the step acquisition stops at the end of the current frame To change the acquisition parameters click the Settings cog on the Acquisition Toolbar to display a dialog You can select Image Scan Size Dwell Time us Input Signal the labels here reflect whatever was set during the installation for example SE BSE or FSD either Con tinuous Scan or Number of Frames and Frame Time secs If your specimen is drifting you can activate AutoLock to ensure that any analysis corresponds to the true loca tion on your image 281 Control Description Mixing Mode Combines signals from the diodes to form a mixed image Some options are available only if the required drop down list l l l diodes are installed and configured FSD only FSD Z Contrast uses upper and side FSD detect
288. inks images You can simultaneously manipulate all the layers using the pan or zoom controls 420 EBSD Description Unlinks images You can manipulate individual layers using pan or zoom controls Use the mouse wheel to zoom in and out of the image Hi Use these tools near the bottom right of the screen to adjust manual and automatic brightness contrast and color Context Menus Right click the electron image to display context menus for copying exporting and printing images See Also Scan Image Toolbar on page 424 Scan Image Settings below FSD dio de controls on page 432 Context Menus Image Viewer on page 157 Export Settings on page 132 AutoLock on page 133 Scan Image Settings The selectable parameters that control image acquisition Image Scan Size Dwell Time and Number of Frames should be chosen according to your specific requirements Both the time taken and the data storage size of the image are dependent on these parameters For a quick look at the specimen select the lowest image scan size and the fastest speed This will enable you to decide whether you require either a higher pixel density in order to observe finer detail such as small features or a longer dwell time in order to improve the image quality by reducing the noise The available acquisition parameters are Image Scan Size Dwell Time us Mains Synchronize Input Signal Software Tilt Correction Contin
289. ion mark icon to select the Show Candidate Element tool Position the cursor at the center of a peak by double clicking with the mouse The list of elements spectra corresponding to the energy at the cursor is dis played in the panel on the right By highlighting an element in this list you will see the markers showing all the lines for this element Note that the Identified Elements will be quantified if you have selected the Current Spec trum or the Fixed List and Current Spectrum Element List in the Quant Settings in the Cal culate Composition step or EDS Quant Settings in the User Profile dialog Note EDS Quant Settings are available in the User Profile Dialog accessed from the Tools menu These settings are also available from the Calculate Composition step Fixed List The elements in the Fixed List are defined in the Quant Settings dialog which is available in the User Profile and the Calculate Composition window Note that the Fixed List is only used for calculating composition in quantitative analysis Example I want to do quantitative analysis on my glass samples and want to compare results from one batch to another batch I am always looking for the same specified list of ele ments You can specify the Element List for Quant from the three available options in the Quant Set tings dialog as shown in the screen shot below 178 EDS SEM OXF INSTRUMENTS The Business af Science Elem
290. ion will only be available if your microscope supports it How can I solve large jumps in the Image If the tracking interval is set too long and the image has drifted significantly then the drift cor rection will be applied in a single jump The result could be seen as a large shift within the image If you see this then set a shorter measurement interval use the Automatic Meas urement Interval or enable Predictive Drift Correction How do the predictive and reactive drift intervals interact The predictive interval Predictive Reference Interval determines how long AutoLock waits between the reference frames when starting predictive drift correction The reactive drift interval Measurement Interval determines how often AutoLock re measures the drift once acquisition starts Generally these settings are independent However if the Automatic Meas urement Interval is enabled the measurement interval won t go lower than the predictive ref erence interval once acquisition has started In most cases where the sample is either fairly stable or settling into stability a good balance of measurement interval vs accuracy should be achievable by using the Automatic Meas urement Interval with a predictive reference interval of up to a minute where applicable What is Drift Proximity 143 Drift Proximity is the potential drift range as a percentage of the field width The proximity display also shows a colored bar
291. is achieved for the unknowns to be determined At this kV the best X ray lines to use for the analysis will be shown Note that you may override the default choice of allowed lines that the Calculate Solubility algorithm uses for each element in the Confirm Analysis step under the Analysis Lines section However in most cases this inter vention will not be necessary The acquisition conditions that the Calculate Solubility pro cedure suggests are indicated by the radio button at the base of the Solubility calculation results section 299 In summary for each predefined kV the calculation works out whether the problem you have setup to calculate is solvable and invertible If these criteria are met Layer Probe then cal culates statistics which then enable the software to suggest the best kV to use based on the Statistics 300 Da O RD FT LayerProbe INSTRUMENTS The Business of Science LayerProbe Settings There are three tabs in the LayerProbe Settings window Quant Setup Model and Analysis Lines Quant Setup The Quant Setup tab allows you to select the deconvolution elements the threshold for quantitative results the correction for detector window artefacts and select quantitative standardizations e Deconvolution elements Deconvolution elements may be used to select elements present in the spectrum that should not be quantified but whose influence needs to be accounted for when
292. isition A relevant section of the image is zoomed and rotated above the Linescan viewer This action aligns the defined line hor izontally to match the x axis of the Linescan viewer Electron Image 1 Display Stacker Settings Line Data 6 ia ie rly 50 f a l ess ERN 2 imm om Minimised Lines Mode _ on The progress of line data acquisition is displayed in Current Site tab in the Data View 4 Element linescans start to populate the Linescan viewer as the data is being acquired 5 You can stop the acquisition by pressing or the red STOP Button To cancel the line processing click the Cancel Processing button in the acquisition tool bar 6 From the controls above the Linescan viewer choose how to process the data for example TruLine 241 The TruLine data processing will use the TruLine settings from the EDS Element settings tab in the User Profile screen You can access the User Profile from the Tools menu You can specifically define whether the threshold is on by selecting Apply threshold for TruLine and entering a Sigma Threshold between 0 0 and 3 0 See Also User Profile on page 22 Acquire Line Data Settings on page 252 242 EDS SEM OXF INSTRUMENTS The Business of Science Displaying and manipulating linescans Three different views are available from the controls in the top right corner of the Acquire Line Data screen Display Electron Image Full Scree
293. isplayed in a single view a Vertical Tiles individual element linescans are displayed in a separate view You can change the height of each view using the Display slider bar Table values for each point on the line You can pan and zoom linescans using the mouse controls Both the viewers image and line view respond synchronously to the mouse interactions a Left mouse button down Move left right pan left right if view is expanded Tip If the list of ele ments and lines obscures the right end of the linescan pan fully to the left Move up down change the scale height Mouse wheel Zooms x range in out around current x value defined by mouse location The image will expand shrink to match the data displayed If the data is not visible in the viewer because of pan zoom state the line on the rotated image will change to a dotted yellow line to indicate there is more data Linescan viewer specifics a Dragging directly on the axis will pan the range Mouse wheel on the axis will expand reduce the range The thickness of the line in the plots can be set globally from the Linescans Viewer tab in the Preferences screen The thickness values in pixels are as tabulated below Thickness in Pixels 393 gt Thickness in Pixels In addition you can change the color and thickness of individual lines from the Settings in the Linescan viewer toolbar 394 EDS TEM OXFO
294. ite Data Tree roject d Specimen 1 4 Site 1 Electron Image 1 4 Point Data 1 FOX EBSD Point 1 spectrum 1 4 Point Data 2 O amp EBSD Point 2 Spectrum 2 Reanalyze Data If you have acquired an EBSD Map with stored EBSPs it is also possible to reanalyze a map region with new settings such as new solver settings or even solving by including different phases Re analyzed map data is stored in the data tree as shown in the screen shot below Data View Current Site Data Tree Electron Image 1 Electron Image 2 Reanalyzed Map Data 2 Reanalyzed Map Data 3 Reanalyzed Map Data 4 Reanalyzed Map Data 5 Reanalyzed Map Data 6 See Also Current Site on page 29 37 Data Tree Menus below Moving data to another PC on page 59 Data Tree Menus Each item such as Project Specimen and Site in the Data Tree has its own menu items Right click with the mouse on a particular item to access the menu entries The menu entries for each item on the Data Tree are described below Project There are two menu items for the Project Remove and Edit Notes Tip Remove removes the project from the Data Tree This option is disabled if only one Project is in the Data Tree Edit Notes opens a dialog for editing Project notes Details opens a dialog showing the Project label and Date time when the Project was created To rename a Project select Save Project As from the File menu Specimen There ar
295. k labels are removed and the spectrum is relabeled according to the User Profile whenever the Element List changes e g when an element is manually added or removed or when AutolD is used s161 Element Lists Any list of elements in the software can be split into the following three categories Pre defined Elements elements expected in specimen Identified Elements typically based on automatic peak identification Auto ID Fixed List used for Quantitative analysis Pre defined Elements You may have prior knowledge of your Specimen and know what elements to look for Examples I want to look for a particular list of elements I am not interested in any other ele ments may want to see their labels on spectra their X ray maps or both I want to see these even if the element is not present I know what s in my sample I want to look for a specific set of elements I want to see these even if the element is not present but I would like to know if there is anything else in my sample too You can define these elements in the Pre defined Elements tab in the Describe Specimen step If you want to save the Pre defined Elements to a profile you must first press Save to Profile button then save the profile via the drop down menu When you want to analyze your Specimen you can load this profile or another profile by pressing the Load Profile but ton in the Describe Specimen step as shown in the
296. l EDS LF Data _ Map Sum Spectrum Mg Kal 2 Ti Keel Cr Kal Min Kal Fe Kal Br Lal EDS Layered Image 1 Electron image This can be a secondary electron image SE or backscatter electron image BSE For EBSD analysis it is generally a forescatterred electron image FSD depending on the detector hard ware installed Map Data EDS and EBSD map data are in their respective Map Data folders As data acquires EBSD maps acquire into the EBSD Data folder If you selected the option to acquire EDS data in addi tion to your EBSD data EDS maps acquire into an EDS Data folder The EBSD Data folder contains the following EBSD images Band Contrast Phase Color Euler Color IPF X Color IPF Y Color IPF Z Color The EDS Data folder contains 455 a Map Sum Spectrum a X ray Element Maps X ray Element Maps Two modes of mapping are available Window Integral Maps and TruMaps Click the appro priate button at the bottom of the maps to select the mapping mode Standard Window Integral maps counts in the energy window are acquired for the element list chosen for analysis These are raw X ray maps which are not corrected for background or peak overlaps You can process the map data as TruMaps which are corrected for background and peak overlaps Post Acquisition Image You can acquire a new scan of the electron image with the current settings after the map is finished by selecting this option under Map acquisitio
297. l sigma and this should be interpreted as fol lows if repeat analyses are performed the observed rel diff value will fluctuate but will typ ically stay within 3 x rel sigma Statistical variation can always be reduced by increasing the Livetime for acquisition or the count rate If you simulate a typical spectrum and quantify it you can see what sort of sigma values you are likely to get in a real measurement and then adjust the acquisition conditions to bring the sigma values within your desired level of accuracy for the measured thicknesses and or concentrations It is impossible to be certain there are no systematic errors but the k ratios provides a useful consistency check If the magnitude of rel diff exceeds 3 x rel sigma this suggests there is Some error in either the theory or the measured k ratios Errors in measured k ratios can be reduced by using standardization in AZtec 288 LayerProbe OXF INSTRUMENTS The Business of Science When a k ratio has a large rel diff with magnitude exceeding 3 x rel sigma this sug gests that there is a systematic error In that case any of the measured thicknesses and or concentrations could be subject to a similar rel diff For example if there is a k ratio with a rel diff of 25 it could be expected that one or more of your determined thicknesses or concentrations could also be subject to a large error In some cases it may be possible t
298. lay as shown below The Confirm Elements window occupies the entire workspace 5 Once you have confirmed the elements you may not require the Confirm Elements window You can remove it from the display if you wish 6 To be able to view the Quant Results switch the Quant Results display on from the toolbar The Quant Results window occupies the entire workspace here Spectrum acquisition and Confirm Elements are switched off from the display The Image Acquisition is dragged on to the second monitor 203 Map Guided ccc In the Guided mode the Map navigator has the four steps The Describe Specimen and Scan Image steps are covered in the earlier section The steps which are unique to this navigator are described here Acquire Map Data 2 2 220 222 cece cece ence eee cece eeee 205 Construct Maps a2 2c ot ie paca EEE EE 219 Analyze Phases 2 2 2 22 2 02222 c ce cee ec ecece eee eee eee eeee ees 226 204 EDS SEM Oy 45O ND INSTRUMENTS The Business af Science Acquire Map Data Acquire Map Data In this step you can acquire X ray maps from the full frame or selected regions of the spec imen The maps show the spatial distribution of all elements in the specimen The results can be displayed as a Layered Image where colors for each element are mixed together and over laid on the electron image or as individual maps Spectra from selected regions can be recon
299. lay the electron image Press to acquire map data or dis play the Layered Image Element Maps The Element Maps component is docked in the top right quadrant of the Acquire and Con struct workspace You can acquire element maps here and view them in three different ways Standard Interactive or Summary view To get details of all the functions follow the Acquire Map Data link below Spectrum Viewer The bottom left quadrant displays the current spectrum It can be a Sum Spectrum or a Reconstructed Spectrum At the top right corner of the Spectrum Viewer there is a link to the Confirm Elements step of the Point amp ID Navigator It is a useful option for identifying and confirming small peaks in the spectrum Select Map to get back into the Acquire and Confirm workspace from the Confirm Element screen Selected Element Details 23 7 The Map Details is located in the bottom right quadrant of the workspace From the Selected Element Details you can select which elements you wish to map You can define the energy windows for window integral maps and select the X ray lines you wish to use for mapping instead of using the automatically selected energy window and lines When you select a map from the element map display the energy window and X ray lines markers for this element are displayed in the spectrum viewer To read details of defining energy windows and choos ing X ray lines follow the link to Construct Maps topic below See
300. layed as you move from channel to channel Acquisition and Settings Toolbar Near the top of the Acquire Spectra window there are buttons for starting and stopping acquisition as shown below Acquire Spectrum START STOP Settings Press the Start button to acquire a spectrum There is a Settings cog in the toolbar For details of settings see Acquire Spectra Settings on page 313 About the noise peak In an X ray spectrum a noise peak sometimes appears near the zero voltage level This small amount of electrical noise is always present from any type of detector Peaks at low energies below 1 keV might indicate various elements such as the Ka line for car bon La line for calcium or Ma line for lanthanum A noise peak can be confusing because it appears to represent an element but has no label You can choose to hide this peak by spec ifying a cut off voltage below 1 keV which removes lower energy values from the spectrum If the noise peak is very high it determines the maximum value for the counts when you reset the spectrum s vertical scale This is shown in the left picture If you exclude this effect you can compare the proportions of elements more easily This is shown in the right picture 101 See Also Excluding the noise peak when resetting scales below Setting the cut off voltage for the noise peak below Excluding the noise peak when resetting scales Note that if the value for the cut off volta
301. le to choose to display the User Interface for example Accessible Theme Light Blue Theme Blue Theme a5 oe Search Tool Enter one or more keywords in the Search Help field near the top right corner of the appli cation window or Help Home Viewer and press The Help Viewer is displayed with links to a list of topics containing the keywords When you click a topic link the topic is displayed in the Help Viewer You can go back to the list of topics by pressing the back arrow near the top left corner of the Help Viewer The keywords are highlighted in each topic To remove all search highlighting click this icon in the toolbar above 54 Getting started ON INSTRUMENTS The Business of Science Color key The color key is an optional feature on many images This key or legend explains the colors For more information hover the cursor over each colored square For example effet 250m To show or hide the color key 1 On the image right click to open the context menu 2 Select View then Color Key 55 FAQs about Software Licensing How can I activate my License Code You will need Internet access to Activate your License Codes If the software is installed on a computer with Internet access you can simply enter the License Code into the License Man ager and press the Activate button The Licence Manager will then automatically send your License Code number to the remote licence server
302. learly display which list is being used A lock icon will be dis played against the Fixed List elements as shown in the screen shot below 194 EDS SEM OXFORD INSTRUMENTS The Business af Science Sum Spectrum Compare In this example Fe and Ti are selected in the Fixed List The rest of the elements in the chart results are from the Current Spectrum because the Element List selected for quantification was Fixed List and Current Spectrum Note that the Fixed List is saved in a User Profile See also Describe Specimen on page 76 Acquire Spectra on page 350 Confirm Elements on page 353 Calculate Composition on page 185 User Profile on page 22 Compare Spectra amp MiniQuant Results Real time Compare and instant MiniQuant options are available in the Acquire Spectra Con firm Elements and Calculate Composition Comparison of Results Two Spectra template steps User can see results without having to move away from the acquisition mode Using these options you can See your results during analysis Compare your current spectrum to a control spectrum during acquisition a View MiniQuant results in a table or a bar chart Click Sl in the top right corner of the Spectrum Viewer in Acquire Spectra Confirm Ele ments or the Calculate Composition window to access the Compare amp MiniQuant options 195 it In the above example Spectrum 1 is the current spectrum and Sp
303. lements 22 02 2 202 e cece cece ee ceeeeceeeeee 353 Calculate Composition 22 222 22222 eee eee eee eee ee 355 Compare Spectra 0 022 e cece eee eee eee ee eee 358 Point amp ID Custom 2 222 222 ee cece ee eee 360 Acquire and Confirm 22 222 22 ecee eee eee eee ceeeeee 361 Map Guided _ 2 2 22 22 o ice ccc eee cee cece cece ecceeceeeees 362 Acquire Map Data 222 222222 e eee cece cece cece eee 363 Construct MANS xe ohn doco inte hand oouienpetekweustocensed 370 How binning affects the quality of your data 373 Analyze Phases 2 222 22 2 2 cece eee e eee cece ee cece ccc ee eee eeeees 375 Finding phases 0 22 2 c cece eee ee cee eee cece cece cess 376 About phase maps 22 2 222 cece eee eee eee cceeeeeee 377 Merging phases 22 22 c eee c eee eee eee cece eee eee 379 Phase maps in the Data Tree 2 2 222 222 eee e ee eee 380 EDS TEM 303 304 Map Custom Analyze Phases settings 0 20 02 cece eee eee eee 381 Analyze Phases toolbars 000 000 cece eee eee eee 383 We gO A Eg eA tse ee ee 386 Acquire and CONS IUCE aces cnc ee ccu chess alodecdon tara cag 387 Linescan Guided 2 2000 22 cece cece ee cece eee eee eee eee 389 Acquiring NINES COINS c lt mos ca matree etree pec aecteuzetaetecends 391 Displaying and manipulating lines
304. lick OK to close the dialog The name of each group appears next to its phases under Phases for Acquisition When these materials have been grouped together band width information will auto matically be used to distinguish phases within a group aay Scan Image Scan Image In the Scan Image step you can acquire an electron image into a Site A Site is like a folder which contains images and analyses for a particular area on a specimen For EDS if you do not want to collect an image and just want to acquire spectra you can skip this step and go straight to the Acquire Spectra step You can have any number of images in a site Just ensure that the images you want to keep are padlocked in the data tree to stop them being overwritten as shown in the screen shot below Data View Current Site Data Tree a O You can toggle between saving or replacing the current image with successive image acqui sition If your specimen is drifting click the Settings cog and activate AutoLock The Scan Image step has several tools for manipulating and enhancing electron images The acquisition toolbar above the electron image and other nearby controls Scan Image toolbar a vertical toolbar on the left for manipulating and annotating the image a Ifa forward scatter electron detector FSD is fitted extra controls are available for combining the signals from each diode into a mixed image Acquisition to
305. load en details aspx id 7 Filtering the list of templates Initially the list on the top right of the dialog shows all the available templates To find a suit able template quickly use the drop down lists in the top left of the dialog to filter the long list and show fewer templates Document Shows only the templates that are in Microsoft Word or Excel Type format Orientation Shows only the templates that have portrait or landscape layout 46 Fe Getting started INSTRUMENTS The Business of Science Menu Description Paper Size Shows only the templates that are suitable for printing ona paper size of Letter or A4 Letter is popular in the USA A4 is popular in Europe Directory Shows templates from all directories or only one directory a System shows the templates as supplied with the software Unless more templates are created you see templates only this directory Current User shows your own templates All Users shows templates you share with other users on the same computer and possibly on the same network Category Shows only the templates that are suitable for images maps or spectra Technique Shows only the templates that are suitable for EDS or EBSD analysis Show Favor Shows only your favorite report templates To mark a favorite ites Only click the star in the column to the left of the title If extra templates have been created for you and other users you might see more t
306. ls on page 214 Optimize Solver Settings You can change the settings for the solver on this dialog Detect Select Edges when the edges of the Kikuchi bands are sharp and clearly visible The band edges are detected based onan initial detection of the peak position in the Hough space and then fine tuning the edge posi tions based on actual EBSPs Select Centers for blurred or narrow bands 447 Number of Bands Determines the number of bands that will be used for initial indexing Increase the number of bands used and this should aid in finding the right solution It is often helpful to look at the Hough and the peak inten sities as this will assist in choosing the number of bands The relation between the number of bands and the number of reflectors is critical in order to get the best per formance of the system It is there fore important to optimize these two numbers Note that too many reflectors can result in more than one solution as can too few bands Experiment with lowering the number of reflectors to optimize your settings Hough Resolution Sets the radius of the area of interest in Hough space in pixels Try dif ferent Hough Resolutions to find the best results for your specimens Use the following guidelines 40 45 For fast data collection where small angular errors lt 2 are not a problem 60 65 A good compromise between speed and angular res olution 75 80 For more accurate
307. lue is determined using the X ray line type K series L series etc for the ratio standard you select For a given X ray line A and ratio standard line R the k factor KAR is calculated as follows KAR a RBR AR Ma Sa Ea where A atomic weight w fluorescent yield Q ionisation cross section and the effi ciency of detector window at that line energy 336 EDS TEM Oy 45O ND INSTRUMENTS The Business af Science Once k factors are known relative to the ratio standard any other k factors can be calculated using the formula k k k AB AR BR You can use any element as you are using theoretically derived k factors Conventionally Si is used Specimen Thickness and Density If you want to apply an absorption correction to the calculated concentration you will need to know the density and thickness of the material The absorption correction is recorded in the Full results section of the quant results Enter the thickness nm and density g cm into the spaces provided These values are then used next time spectra are quantified To recalculate the current analysis with different values edit the required value and go to the Calculate Composition step Threshold Quantitative Results Quantitative results are displayed with value which is one sigma standard deviation based on counting statistics Typically results which are less than 3 sigma have reduced sig nificance and so it may be desirabl
308. lysis folder in All Programs on the Windows Start menu a Select Open Project from the File menu on the menu bar Browse to the Project folder Select the Project file with oip extension and press Open The Project is loaded and the data items are populated in the Data Tree 59 Getting Help The Business af Science Getting Help Various elements of Help available in the software are described below e Context Sensitive Help F1 The active workspace in the application has an associated help topic Press F1 to access the help topic Each help topic has useful links for further information e Step Notes A default editable set of notes are provided for each navigator step The user can then overwrite these or add notes as required A reset to default settings is avail able e On Line Help There are six options available from the Help menu on the application menu bar A Show Help F1 This opens the Help Viewer with TOC in the left pane and the help topic on the right You can also launch the Help Home Page by pressing u in the top right corner of the application window The Home Page has the facility for searching the Help by entering the key words in the search field It has links to the following four help items Getting Started This opens a page with links to topics to give you information about the main fea tures of the user interface and Frequently asked questions about the software licens
309. m User Standards Standardizations file defined by the user Pulse Pile Up Correction Enabled Disabled Detector File Indicates file that has been used to char acterize detector Efficiency Calculated File based Quant Results View The information displayed in the Quant Results View depends on which template has been selected You can view Spectrum Details Soectrum Processing and Diagnostics table in addi tion to quant results See Also Quant Settings below Element Lists on page 191 Compare Spectra amp MiniQuant Results on page 195 Quant Settings The Quant Settings are described below Processing Options To make the correct selection a little knowledge of the specimen is required For example can all elements in the specimen be detected and analyzed or are you analyzing a mineral where it is more usual to calculate the oxygen present e All Elements 187 This option is used when processing spectra from specimens in which all elements yield X rays which can be readily detected e g steels alloys and other materials with insignificant amounts of elements lighter than sodium e Element by Difference This option can be used if you can readily measure X ray signal from all elements except one in the specimen The omitted element is called the combined element The concentration of the combined element is not measured but it is calculated assuming that the difference between the analyzed total and 100 is du
310. m 2 J z Project Project is a top level container for data Each Project is associated with a folder on the file sys tem The name of the folder is the same as the Project name The Project folder contains a sin gle file with an oip extension and optional Data and Reports sub folders Note When moving or copying project data ensure that the root project folder is moved copied not just the oip file The folder can be zipped using the standard Win dows compression utilities if required Specimen Specimen represents the real specimen that you analyze and collect the data from including images maps and spectra There may be many Specimens in a single Project A Specimen may contain more than one Site N Site Site represents an area on the Specimen from where you acquire data such as images spec tra and maps Site can hold multiple images for example SE and BSE plus any imported images 86 EDS SEM Oy 45O ND INSTRUMENTS The Business af Science The analytical conditions such as kV Magnification and Calibration are stored with the data Electron Image Electron Image on each Site can be a secondary electron SE image a backscattered electron BSE image or a forward scattered electron image You can acquire two images simul taneously if suitable hardware is available FSD Data This folder is the container for all FSD data It contains electro
311. m of coating with carbon is using evaporation A high current is passed through carbon rods under vacuum The heating effect causes the carbon to evaporate and in turn this is deposited as a thin film on the surface of the sample The actual process of formation of a thin film is a complex process and not fully discussed here Ensure that one of the carbon rods is sharp The end of one rod is usually flattened while the other will be pointed Place your sample in the evaporator Evacuate the chamber Once the desired vacuum has been achieved usually about 1x10 Pa it is important to out gas the rods This is done by heating them until they glow a dull red The pressure in the chamber will rise and the pressure should then be restored before the evaporation process Pass a high current through the carbon rods 80 OXFORD J er INSTRUMENTS The Business of Science The heating effect causes the carbon to evaporate and deposit a thin film on the sur face of the sample It is often useful to place a piece of white paper or filter paper beneath the sample to help you gauge the amount of carbon you deposit Although the degree of coating you need will depend on the conductivity of the sample as rule of thumb when the paper appearance of the paper becomes light brown this should be sufficient carbon Element Lists Any list of elements in the software can be split into the following three cat
312. mage for detailed description read the topic Modes of X ray spectrum acquisition on page 150 The screen shot below shows the defined points and areas on the image and the spectra being populated on the Data Tree Gh te perenne thule Propi Li 2 ee ohran lob Frp k i hmo hem Pal a ir rep pa re eee Qe Ferr ha mpri appn ope Tja oy el ede ui om le mpira 2 FESSA E re ee 7 i io a oh ih led Pham DDS ried Aee OS ys Spectra have been acquired from the areas and points white labeled as Spectrum 1 2 and 3 Spectrum 4 is currently being acquired from the area yellow labeled as Spectrum 4 Spec trum 5 blue is in the queue For step by step guidance on how to acquire spectra see below Spectrum acquisition from a single point a Having acquired an image in the Scan Image step navigate to the Acquire Spectra step Select the Point Tool from the Toolbar on the left of the window Click on the image with the mouse to acquire spectrum from a point 148 ON EDS SEM INSTRUMENTS The Business of Science Spectrum acquisition starts from that point The position of the point is marked as a cross on the image and it is labeled as Spectrum 1 It is added to the Data Tree just below the image it is acquired from The progress of spectrum 1 acquisition is displayed on the Current Site tab Spectrum acquisition from multiple points Having acquired an image in the Scan Image step navig
313. mage and show acquisition areas and select the highlight reanalyzed areas The image viewer will display all the Reanalyzed maps i e band contrast Euler IPF maps Electron image and post acquisition image It is worth noting that you can only reanalyze one map at a time All reanalyzed map data will be saved in the data tree To see all your map details highlight and right click on the EBSD data folder Notice the Parent EBSD Map details will reference your reanalyzed map data project name Deleting Maps Reanalyzed maps are dependent on the processed patterns of the original map dataset To delete a reanalyzed map from the analysis completely simply go to the data tree right click and delete Therefore all folders located in the Reanalyzed Map data folder will be deleted Therefore deleting the processed patterns from the original map dataset with reanalyzed maps remaining in the data tree will prompt an error message The error message will warn you All references to the stored patterns would be deleted Without patterns it is not pos sible to reanalyze the data any further Delete emis A Are you sure you would like to delete the selected item s All references to the stored patterns will be deleted No Creating a Pole Figure Pole figures represent the orientation distribution of lattice planes in crystals and textures of materials You can construct a pole figure after you have acquired map data 1 On th
314. mage with Colour Spectrum and MiniQuant System Layered Image Colour Spectrum Categon Maps Technique All Layered Image and Maps System Layered Image Maps A4P dock Layered Image with Multiple BAW Spectra and no MiniQjuant System Layered Image Multiple BW Spe E Show Favorites Only Layered Image with Multiple BRW Spectra and MiniQuant System Layered Image Multiple BW Spe Layered Image with Multiple Colour Spectra and no MiniGQuant System Layered Image Multiple Colour Layered Image with Multiple Colour Spectra and MiniQuant System Layered Image Multiple Colour Maps F System Maps A4 P doc System AA Pi xlsx System Maps AFP xlsx Template Generator System Maps A4P dock Maps P Set As Default Close If Microsoft Word or Excel is installed on your computer the lower part of the dialog shows a preview of your report You can click on the title of any report in the list above it to see dif ferent layouts To change the magnification right click the preview and use the context menu Note that the preview works only if your version of Microsoft Word can save a document as XPS format Office 2010 is supported but Office 2003 Is not For Office 2007 see the File menu option Save as If your Office 2007 does not have the XPS option you can copy a plug in from the product DVD in folder Customer Support Office2007 Alternatively you can down load from http www microsoft com down
315. mall differences may be obscured by statistical scatter The smooth function applies an energy dependent filter to the spectrum This has the effect of slightly broadening the peaks and also filtering out the rapid fluctuations due to statistics Statistical fluctuations can sometimes appear like a real peak When it is difficult to decide whether a peak is present or not the smooth function substantially reduces the statistical fluctuation so that any real peak becomes more visible Siz ls Analyzer Custom Analyzer is microscope centric application X ray spectra are acquired from the regions on the specimen scanned by the microscope beam There are two modes of operation in the Analyzer application Guided and Custom In the Custom mode the Analyzer navigator has three steps The Describe Specimen and Compare Spectra steps are explained in the previous section The new step is described below Acquire and Confirm 0 00 00 0222 ccc c cece ccc eee ee cece eee ee eeee 123 122 EDS SEM The Business of Science Acquire and Confirm Acquire and Confirm Acquire and Confirm is the main step of the Analyzer Navigator in the Custom mode Three components are available in the single workspace The Acquire Spectra component is located in the top half of the workspace Quant Results in the bottom left and Confirm Elements in the bottom right The three components are combined in the Custom mode to give you
316. map The reanalyze toolbar allows you to reanalyze a region of the complete map or entire map by selecting a rectangular elliptical or free hand region Select your desired shape region to reanalyze your EBSD map Click Start to start reanalysis Please take note that your total Area number of pixels will be dependent on the selected region x During reanalysis your Data Tree will display your data and map statistics under the E Reanalyzed Map folder Note that the processed patterns folder will also be stored under the Reanalyzed Map Data folder each time a map is reanalyzed The reanalyzed map in the data tree is the original project map area plus the selected region of reanalyzed pixels All reanalyzed EBSD and EDS map data will be displayed in the data tree Results of Data Reanalysis EDS and EBSD data Reanalysis of reanalyzed maps with both EDS and EBSD data is possible and the EDS data can be viewed together with EBSD reanalyzed maps Note that the EDS data under the Reana lyzed Map is a complete copy of the original EDS data Select your reanalyzed map on the data tree and the electron image of your choice will display the phase key for phases only identified during the data reanalysis You can then change additional acquisition settings and start reanalysis of the reanalyzed maps Different regions analyzed 467 You can overlay all your reanalyzed map regions on the electron image Simply right click on the electron i
317. matically change the settings in the other Why do we need to perform Beam Meas urement The microscope beam current may vary with time If we want to measure absolute concentrations we need to make a comparison of intensity of a peak with that from a known material If we measure a known material we can then make accurate intensity measurements on unknowns provided the beam current doesn t alter after the optimization How often should I perform Beam Meas urement Ifyou wish to calculate un normalized totals the frequency with which you perform the optimization will depend on the stability of the beam current Repeated meas urement of a known standard will indicate whether the beam current is varying The variation in the analysis total will be in direct proportion to the change in current since the last optimization How to perform Beam Measurement The Beam Measurement routine requires the acquisition of a high quality spectrum from a suitable element from which details of the beam current is calculated and stored One ele ment can be used for both the Beam Measurement and Energy Calibration or you can use two different elements if you wish To perform Beam Measurement follow the steps 68 EDS SEM Oy 45O ND INSTRUMENTS The Business af Science Select a calibration routine from the drop down list of Energy Calibration and Beam Measurement Select an element from the Calibration Element drop
318. mbining signals from several neighboring points the binning technique produces an averaged signal which has less noise overall The effect is similar to collecting the original data at a lower resolution and a longer dwell time You can select the binning factor from the drop down list below the map or linescan display Effect of binning on element maps A binning factor of four combines 16 adjacent pixels from each 4x4 square into one new pixel For example 71a EDS SEM Oy 45O ND INSTRUMENTS The Business of Science Binning is useful when you are using the TruMap mode for mapping because of the improved statistics Binning also enables AutoLayer to combine similar maps more suc cessfully because of the lower noise See also AutoLayer on page 222 Effect of binning on linescans Binning combines a group of pixels into one new pixel The binning appears to shorten the linescan at each end In the following example with a binning factor of 16 the first value appears at approximately 8 um because the first binned point is midway between the first 16 values 12000 12000 11000 11000 10000 9000 10000 9000 8000 7000 g000 7000 6000 5000 4000 3000 2000 1000 U LL DA faa es ba are Say iy 32 36 40 n E ee es Li i r i E E Original data at 1 um spacing Binned data 215 Layer modes in the Interactive map dis
319. me 1 is the shortest and as such gives the highest X ray acquisition rates but at some cost to resolution Process time 6 is the longest and gives the highest resolution but at some cost to maximum acquisition rate The longer the Process time the slower data can be acquired i e the higher the system Deadtime will be for a given input count rate The input rate is not affected by the pulse processor 213 Pixel Dwell Time ps The default value for dwell time per pixel is 100 us Frame Live Time s The value of frame live time depends on the map resolution and pixel dwell time Brightness Contrast and Gamma Controls You can adjust the brightness and contrast of the currently selected image or map Press lt on the Display toolbar to open the Brightness and Contrast dialog Auto Brightness and Auto Gamma Using the Auto brightness and Gamma buttons on the bottom right hand corner of the Map display window allows you to change the Brightness Contrast and Gamma for all the maps The Auto Brightness button optimizes the maps to give the best Layered Image and the Auto Gamma enables you to see all the map data including background noise How binning affects the quality of your data As the electron beam scans a line or area of the specimen data is acquired from numerous points Inevitably the signal from each point includes some noise If data is not acquired for long enough the noise level will be high By co
320. men Geometry and Phases via the links below See Also Specimen Geometry below Phases on page 416 Data Tree on page 85 Mini View on page 93 Step Notes on page 94 Specimen Geometry Specimen Tilt This area of the application allows you to define the way that the Specimen is tilted in the chamber with respect to the horizontal plane Diffracted electrons only escape from a depth in the order of a few tens of nanometers deep from the sample surface At low tilt angles the total interaction volume close to the surface is very small compared to the interaction volume deep within the material Consequently at zero or low tilt the proportion of diffracted electrons in the overall electron yield may be so low as to be undetectable Tilting the sample improves the diffracted component to back ground yield ratio by increasing the volume of near surface material excited Thus EBSD is gen erally carried out at approximately 70 degrees tilt Pretilted Specimen Holder If you are using a Pretilted Specimen holder for your experiment check the corresponding box and enter the corresponding Tilt Angle Note that this option is only enabled in the appli cation if it has been checked in the Configuration Tool under Enable Software Features in Application If you are not using a pretilted holder this angle will be zero Remember to switch off the Pretilt option when you are not using a pretilted holder since it will affect EDS and EBSD data
321. mmary and Pre defined Elements Summary In the Summary view you can write notes on the Project and the Specimen present in the Project For convenience you can also copy images diagrams and text from other doc uments emails and paste into these windows Notes are saved with the Project and you are allowed to edit notes in any step of the Navigator It helps to capture the important infor mation during the analysis Click with the right mouse button on the Project or Specimen in the Data Tree and then select Edit Notes to write modify the relevant notes You can add new Specimens to the current Project by pressing the New Specimen button New Specimen Specimen 1 Click on the Specimen in the Project Overview dialog This action displays the Specimen Notes for Specimen 1 text box Here you are provided with the text formatting tools You are allowed to write notes about each Specimen and save them Pre defined Elements If you know what elements are present in your Specimen and you only want to see peak labels or X ray maps for those elements then you can select them in the Pre defined Ele ments tab Press the Pre defined Elements tab to access the periodic table If you wish to enable the AutoID option check the Perform AutoID During Acquisition option 310 CX FORD EDS TEM INSTRUMENTS The Business of Science Summary Specimen Geometry Pre defined Elements Pre defined Eleme
322. n Display Linescans and Electron Image s Display Linescans Full Screen Ole se Several options are available to view the Linescans a Stacked multiple linescans overlaid are displayed in a single view a Vertical Tiles individual element linescans are displayed in a separate view You can change the height of each view using the Display slider bar Table values for each point on the line You can pan and zoom linescans using the mouse controls Both the viewers image and line view respond synchronously to the mouse interactions a Left mouse button down Move left right pan left right if view is expanded Tip If the list of ele ments and lines obscures the right end of the linescan pan fully to the left Move up down change the scale height Mouse wheel Zooms x range in out around current x value defined by mouse location The image will expand shrink to match the data displayed If the data is not visible in the viewer because of pan zoom state the line on the rotated image will change to a dotted yellow line to indicate there is more data Linescan viewer specifics a Dragging directly on the axis will pan the range Mouse wheel on the axis will expand reduce the range The thickness of the line in the plots can be set globally from the Linescans Viewer tab in the Preferences screen The thickness values in pixels are as tabulated below Thickness in Pixels
323. n Data Tree 229 380 phase viewer default display 14 phases 3D view 416 cannot remove 417 database 416 grouping 417 in EDS data 226 227 375 376 pole figure 468 viewer 15 predictive correction 140 preferences 13 reports 18 48 process time 71 213 profile user 22 project file 29 folder 59 transfer to another computer 59 Q qualitative analysis EDS 73 R Report Template Generator 51 report templates changing 52 reports change logo in 51 context menu for templates 50 for many sites 49 generating your own template 51 on the fly 50 preferences 18 48 printing 44 quickly create a 50 send by email 44 site 44 template preview does not work 46 503 templates Resolution S Search help search tool Smooth specimen geometry specimen tilt spectrum default view spreadsheet linscans standardization status bar Step Notes support panel T Themes tilt specimen toolbar Scan Image Tools menu tree data U user interface user preferences user profile V View menu W Welcome Screen working distance Z zoom on electron image 504 45 145 157 212 223 448 457 62 54 17 121 339 359 414 414 16 250 400 263 265 267 19 20 27 61 2 10 53 414 130 424 10 30 85 13 22 19 494 131 424 Index O45 O ND INSTRUMENTS The Business of Science 505
324. n different ways according to the result type For example if the result type is Atomic fraction then Sodium Chloride NaCl will be shown as Na0 50CI0 50 If the result type is weight fraction then the composition will be shown as Na 0 61 CI 0 39 Note the use of square brackets when describing weight fraction Result Type spectrum 1 Atomic Fraction Compare Atomic Fraction i Weight Fraction 574 nm Substrate 5 Atomic Fraction Comparing spectra 285 The current spectrum can be compared with another spectrum in the Data Tree from the same project or from another project The compare spectrum can be chosen via the Compare drop down The selected spectrum is overlaid on the current spectrum as a line spectrum It is a very useful feature for visually identifying any differences in the spectra See Also Acquire Spectra Settings on page 313 Acquire Spectra Toolbar on page 151 Calibrate on page 66 Brightness Contrast and Gamma Controls on page 214 Context Menus Spectrum Viewer on page 321 286 LayerProbe Oy 45O ND INSTRUMENTS The Business af Science In this step the thickness and composition values for the model structure defined in the Describe Model step are calculated from the experimental data selected in the data man agement using the nominal values of the unknowns as starting points The quality of the solu tion can be assessed visually by overlaying the theoretic
325. n images from each diode and the FSD mixed image which is the result of combining some or all of the FSE images S FSD Data 2 sh Folder of images 3 FSD Channels Upper Left 3 Image from a single FSD diode Upper Right 3 Lower Left 3 Lower Right 3 Side Left 3 Mixed image Side Right 3 SD Mixed Image 3 Imported Image Any standard Windows Picture files can be imported into the Project for comparison or reporting The file formats available are JPG JPEG BMP PNG WDP GIF TIF and TIFF You can import an image using the context menu available from the Site Spectrum Spectra are acquired from the areas defined on an electron image Sum Spectra and Recon structed Spectra are shown under the Map in the Data Tree You will see the following items in the Data Tree if you are acquiring element maps in the EDS application 87 Data View Current Site Data Tree So d q Specimen 1 4 lt gt Site1 Electron Image 1 a Map Data 1 4 EDS Data Map Sum Spectrum Mg Kal _2 Ti Kal Cr Kal Mn Kal EDS Layered Image 1 Map Data 7 EDS Data Map Sum Spectrum Mg Kal_2 Ti Kal Cr Kal Mn Kal EDS Layered Image 2 Mineral imported image Map Data Map Data is the container for a mapped area s in a Site It can hold EDS Data EBSD Data or both One Site can contain more than one Map Data items In the example above there are two items Map Data 1 and Map Data 2 EDS Data EDS
326. n settings This is useful for checking drift of the specimen Tips Hover the mouse over the Map Data entry on the Current Site to see the acquisition progress and information such as speed and hit rate To delete a map from the analysis completely right click it to access the context menu on the Data tree or Current site Reanalyzing Map regions If you have acquired an EBSD Map with stored EBSPs you can reanalyze a map region with new settings Setup the required phase and solver settings in previous steps then use one of the reanalyze tools to select a smaller area 1 In the toolbar on the left of the layered image click an icon then outline the region Outlines a rectangular or square feature or area on an image Outlines an irregular shaped feature on an image Outlines an oval or elliptical feature on an image 2 Click and drag the mouse on the image to outline the area 456 EBSD Oy 45O ND INSTRUMENTS The Business af Science 3 Release the mouse button The map data will be reanalyzed from it Reanalyzed map data is automatically stored in the data tree as shown below Data View Current Site Data Tree Electron Image 1 Electron Image 2 Reanalyzed Map Data 2 Reanalyzed Map Data 3 Reanalyzed Map Data 4 Reanalyzed Map Data 5 Reanalyzed Map Data 6 See Also Context Menu Map Viewer on page 223 Acquire Map Data Settings below Display Modes and Map View Setti
327. n the image Data View Current Site Data Tree y Epp a Specimen 1 4 Sitel Electron Image 1 4 F Point Data 1 re EBSD Point 1 spectrum 1 4 Point Data FOE EBSD Point 2 Spectrum 2 Reanalyze Data oye EDS SEM Oy 45O ND INSTRUMENTS The Business af Science If you have acquired an EBSD Map with stored EBSPs it is also possible to reanalyze a map region with new settings such as new solver settings or even solving by including different phases Re analyzed map data is stored in the data tree as shown in the screen shot below Data View Current Site Data Tree Electron Image 1 Electron Image 2 2 Reanalyzed Map Data 2 Reanalyzed Map Data 3 Reanalyzed Map Data 4 Reanalyzed Map Data 5 Reanalyzed Map Data 6 See Also Current Site on page 29 Data Tree Menus on page 38 Moving data to another PC on page 59 Mini View The Mini View is an area of the Support Panel dedicated to the display of a number of dif ferent views which you can select depending on what data you wish to view Views con taining the current Electron Image Spectrum Monitor or EDS Ratemeter are examples of such views Electron Image The full field of view of the currently selected electron image is displayed here It is often use ful to refer to this image in steps where your application area is dedicated to displaying spec tra or maps For example you can view the electron image in the Mini View if yo
328. n the left are available to assist you in con firming elements manually For details see Confirm Elements Tools on page 174 Once all elements in the spectrum have been identified and confirmed you can email the spectrum to your customer or generate a Microsoft Word or Micro soft Excel report using the Export option available on the context menu on the Spectrum viewer For further details of context menus available on the Spectrum viewer see Context Menus Spectrum Viewer on page 321 You can use the confirmed element lists to acquire element maps and linescans and perform quantitative analysis Confirm Elements X within the Construct Maps and Construct Linescans steps to confirm an element for map and linescan acquisitions 74 EDS SEM The Business of Science Analyzer Guided Analyzer is a microscope centric application X ray spectra are acquired from the regions on the specimen scanned by the microscope beam There are two modes of operation in the Analyzer application Guided and Custom In the Guided mode the Analyzer navigator has five following steps Describe Specimen _ 2 2 2 2 222 c cece cece cece cece ccc ceecceeeeceeees 76 Acquire Spectra 2 222 022 0222 c eee ccc cece cece cece cece ceeeeceeeeeees 96 Confirm Elements 2 222 002 coe e ee eee ee cee ccc eecceeecceeeeceeeees 115 Calculate Composition 2 2 022 022 2c cece cece eee ce eee ceeeeeees 117
329. nce and the number of Kikuchi bands using the options on the 3 D Phase View context menu by selecting a different kV and Simulator Reflectors The unit cell visualization gives a 3 D simulation of the unit cell of the selected phase with the a b and c axes marked respectively in red green and blue Using the mouse you can freely rotate this simulation Phases for Acquisition In the list of Phases for Acquisition it is possible to include exclude individual phases When the phase is not included that phase will not be used by the software for indexing EBSPs The number of reflectors per phase used during indexing can be adjusted by selecting the appropriate number from the drop down list This number tells the software how many theo retical Kikuchi bands to utilise during the indexing process Lower numbers generally result in faster indexing but may also give a lower hit rate of EBSPs indexed and more wrong or misleading solutions If you wish to add a phase froma cry or hkl file to the Phases for Acquisition list press the Add from File button 416 EBSD The Business of Science Once you have acquired the EBSD data into a Specimen you can not remove phases you can only add them However you can disable them this is to ensure data coherent in a Specimen for future applications See Also Configuring groups of phases below Configuring groups of phases During EBSD analysis there are some
330. nd Ti are selected in the Fixed List The rest of the elements in the chart results are from the Current Spectrum because the Element List selected for quantification was Fixed List and Current Spectrum Note that the Fixed List is saved in a User Profile See also Describe Specimen on page 76 Acquire Spectra on page 350 Confirm Elements on page 353 Calculate Composition on page 185 User Profile on page 22 Data Tree Data is archived in a logical manner and can be directly viewed via easily recognizable icons on the Data Tree To access the Data Tree select the Data Tree tab on the Data View panel All open Projects and their contents are displayed in the Data Tree Multiple Projects can be opened and shown in the Data Tree at the same time If you have multiple Projects Spec imens or Multiple Sites in the Data Tree you can easily get to your current site by pressing the Current Site tab When the application is started a default Project containing a Specimen and a Site is shown As you acquire data items are added to the Data Tree The current items in the Data Tree are shown in bold Click on an item on the Data Tree to make it current Items on the Data Tree 20b The screen shot below shows an example of the main items in the Data Tree Each item is described along with their icons below Data View Current Site Data Tree Project 1 k Specimen 1 4 C Sitel _ Electron Image 1 Spectrum 1 Spectru
331. nd its search range in the Phase Search if the minimum con centration of the element is greater than the threshold value set Optional This means optionally include this element and its search range in the Phase Search if the minimum concentration of this element is less than the threshold value set Exclude ATS EBSD The Business of Science This means exclude the element and its search range in the Phase Search Wild Cards A number of wild cards can also be used in the search which means that you are including 0 1 2 unknown elements during the search You should also note that adding wildcards can significantly slow down the search process of the database As an example a search using Ti and one wildcard will find Ti as well as all combinations of Ti and one other element such as TiC and TIN Conducting the Phase Search A list of available databases is shown Check the databases you wish to search through and press Search The results of the Phase Search are shown in the Phase Search Results table The name of the phase the database from which it was found the Space Group and the Com position are all reported in this table If you wish to limit the search to fewer databases uncheck the database and press Search again After performing search the list of found phases are now stored associated with the highlighted spectrum This will be used in the next step Databases User created databases can also be
332. nd prints it imme diately on your default printer As an alternative you can use Save As and print the document later Sends the report using the default email package installed on your com puter The following menu options affect site reports and report templates Menu option Description Site Report Generates a report about every type of information taken from the site You can choose the format Word or Excel paper size and file location if Microsoft Word or Excel is installed Report Templates Shows a list of the available templates See the next section about the Report Templates dialog Report Templates dialog Reports are generated from the templates which determine the look and feel of the final report A set of templates are provided with the software These templates include items which you might like to save print or email for example Quant Results and Spectra You can view the complete set of templates by clicking the down arrow on the Report Results button then selecting the Report Templates option 45 Report Templates T Document Type All Title Directory File Orientation Layered Image with B amp W Spectrum and no MiniQuant System Layered Image BW Spectrum n Layered Image with B amp W Spectrum and MinitQuant System Layered Image BW Spectrum w Layered Image with Colour Spectrum and no MiniQuant System Layered Image Colour Spectrum Paper Sime AA Directory All Layered I
333. nding on your microscope magnifications of up to 300 000 can be attained However above these magnifications no greater detail is observed because of the size of the scanning probe Any greater magnification is often referred to as empty magnification Element Mapping If you are acquiring X ray data from a point choose a magnification so that you see sufficient detail to allow you to position the beam Choosing a magnification greater than 1000 times will usually ensure that you are analyzing in the center of the field visible to the X ray detector and will allow you to scan over this area to obtain a map Note that the beam diameter is usually much smaller than the excitation volume so that even if you position the beam on a small feature in an electron image the X ray data that you obtain may originate from the surrounding material 497 Index The Business of Science Index A Accelerating voltage 299 439 494 496 Analyze Phases Boundary Tolerance 230 381 data tree 33 89 Grouping Level 231 382 left toolbar 234 385 map display tools 232 383 name order and number of phases 227 377 process settings 230 381 toolbar 232 383 what is a phase 226 375 window areas of the 226 375 annotation on electron image 131 424 Auto ID Confidence Factor 25 auto save 14 AutoLayer vil 207 215 222 224 365 373 453 AutoLock Drift correction 125 128 133 138 140 280 346 418 422 AutoPhaseMap 226 375 B be
334. ne the area the calculator changes the step size While you define the step size the area changes to keep the time constant 450 EBSD The Business of Science Icon Description Step Size Locks the step size While you define the area the calculator changes the duration While you define the duration the acqui sition time changes to keep the step size constant Area Width Locks the width of acquisition area While you define the acquisition time the calculator changes the step size While you define the step size the acqui sition time changes to keep the area con stant ES Fixes the width to height ratio of the map area Any change in one direction automatically causes a change in the other direction If you maximize the area to be mapped the current aspect ratio setting is ignored and then recalculated for this new area Fills the field of view with as many points as possible using the defined step size Repositions the area to be mapped to the center of the field of view Moves the acquisition area Click in the middle of the area and move the mouse Resizes the area If you have not locked the area you can resize it by clicking and dragging the edges Select the acquisition parameters from the Settings cog on the acquisition toolbar and click Start to acquire the map Defining a map region using the standard region tools By default map data is acquired from the full area To acquire
335. nergy Range keV Select a spectrum energy range from the available options of Auto 0 10 0 20 or 0 40 keV from the Energy Range drop down list The appropriate energy range should be selected in conjunction with the current microscope accelerating voltage If the accelerating voltage is above 10 kV in order to view lines which may be excited above 10 keV the 20 keV range should be chosen Below 10 kV it may be more appropriate to choose the 10 keV range since no lines above 10 keV will be excited In the Auto mode the system checks for the accelerating voltage set on the microscope and selects a suitable energy range in the software Process Time Select the Process Time from the drop down list of Process Times Default and 1 to 6 The Proc ess time Is the length of time spent reducing noise from the X ray signal coming from the ED detector during processing By selecting different Process times it is possible to reduce dif fering amounts of noise The longer the Process time the lower the noise If noise is mini mized the resolution of the peak displayed in the spectrum is improved in other words the peak is narrower and it becomes easier to separate or resolve from another peak that may be close by in energy If Default is selected the Process Time is automatically set to a suitable value There is a trade off between the Process time that is used and the speed at which data can be acquired into the X ray spectrum Process ti
336. ng navigators in the software Analyzer Guided on page 75 Analyzer Custom on page 122 Point amp ID Guided on page 124 Point amp ID Custom on page 199 Optimize on page 262 Map Guided on page 362 Map Custom on page 386 Linescan Guided on page 389 Linescan Custom on page 406 EBSD Map on page 412 Phase ID on page 473 Menu Bar There is a menu bar at the top of the application window containing several menu options Each menu has several items which are described below File View Techniques Tools Help File on the facing page View Menu on page 9 Technique selector on page 9 Tools Menu on page 10 Help on page 12 The Business of Science File Menu Getting started Menu Description New Project Open Project Remove Project Save Project Save Project As Removes any existing Projects prompts to save and then opens a new Project as Project de Removes any existing Projects from the data tree then opens an existing Project prompts to save any existing Projects if required New Project Adds a new Project and leaves any open Projects in the data tree New Specimen Adds a new Specimen in the Project that has focus New Site Adds a new Site in the Project that has focus Existing Project adds an existing Project and leaves any open Projects in the data tree Removes the highlighted Project If there is only one Project in the data tree the Remove
337. ng the thickness of each layer 1 Select either Unknown or Fixed thickness 2 If Unknown thickness is selected enter the thickness in nm 3 Specify a percentage tolerance to be applied to the nominal thickness during anal ysis Note that the tolerance of the nominal thickness is a relative not an absolute parameter For example if the layer thickness is 40 nm a tolerance of 15 will allow the thickness to be 40 6nm Once the composition and thickness of a layer in a structure is defined it is displayed in a table on the left side of the workspace under the Model The thickness in nm is displayed in the first column Then the composition is shown with each element symbol followed by its atomic fraction 278 LayerProbe OXF INSTRUMENTS The Business of Science Model Thickness nominal Composition nominal Add Above 38 00 nm Al pao oso Add Below Substrate Si Move Down Delete Clear All Import Export Restore Save Model If a model already exists tfe or tff file you can import it by pressing the Import button a tfe files are ThinFilmID specific a tiff files are Stratagem type files that can be used in ThinFilmID and in LayerProbe You can also export your model to a file allowing the use of existing models and the sharing of settings between systems Once the model is defined save it by pressing the Save button The model is stored in the cur rent User Profile settings and can be r
338. ngs on page 460 AutoLayer on page 222 Storing EBSD patterns without solving on page 459 Acquire Map Data Settings Resolution The resolution of a map is defined as the number of picture points or pixels along the x and y axes e g 256 x 256 512 x 512 or 1024 X 1024 The quality of the image improves as the res olution at which an image is acquired is increased A microscope monitor CRT is usually a rec tangular display rather than square so the resolution is displayed as a rectangle i e 256 x 200 in order to take into account the aspect ratio The y dimension is set at installation when imaging is calibrated and it will vary from system to system Select a resolution for Map acquisition from the following options available 64 x 64 128 x 128 256 x 256 512 x 512 1024 x 1024 2048 x 2048 457 4096 x 4096 Step Size nm This is the size of the spacing between beam acquisition points If you wish to use a different step size to the one determined by the imaging resolution type in the required step size The software will not permit the step size to be smaller than the step size corresponding to 4096 x 4096 resolution Similarly it must be larger than the step size corresponding to 64 x 64 res olution Store Patterns During map acquisition you can choose the storage conditions for the EBSD patterns Select an option All Patterns solves and stores EBSPs in the project Zero Solutions stores only those
339. nnels Select number of channels from the drop down list of Auto 1024 2048 or 4096 4K with which you wish to display the spectrum The number of eV channel will depend on both the energy range and the number of channels you select Energy Range keV Number of Channels eV channel In the Auto mode the system checks for the energy range selected and sets the appropriate number of channels 154 4760 FD er INSTRUMENTS The Business of Science Note The Energy Calibration routine is performed for all process times and for all available energy ranges and number of channels It means if you change any of these settings soon after you had performed the Energy Calibration you do not need to re optimize the system Process Time Select the Process Time from the drop down list of Process Times Default and 1 to 6 The Proc ess time Is the length of time spent reducing noise from the X ray signal coming from the ED detector during processing By selecting different Process times it is possible to reduce dif fering amounts of noise The longer the Process time the lower the noise If noise is mini mized the resolution of the peak displayed in the spectrum is improved in other words the peak is narrower and it becomes easier to separate or resolve from another peak that may be close by in energy If Default is selected the Process Time is automatically set to a suitable value There is a trade off between the Proce
340. ns even scratches in the phosphor The background does not have to be calculated for each EBSP acquired Disadvantages The background is likely to change position and magnitude when the Position of the detector changes Position of the Specimen changes in the chamber Mean atomic number Z changes significantly in a multi phased material Position of the electron beam changes on the specimen surface at low magnification Accelerating voltage is changed Stage tilt angle is changed Note that any changes to gain binning or exposure time mean that a new static background should be collected Auto Background Check the Auto Background routine option to background correct the acquired EBSP s on the fly The Auto Background process is very efficient at preserving the original shape and features of the data such as the Kikuchi bands whilst removing the unwanted background Advantages Seamless process requiring no user intervention Independent of acquisition conditions Disadvantages a The dynamic correction is per EBSP slower than the static one because the back ground has to be calculated for each pattern It cannot compensate for local irregularities in the sensitivity of the phosphor Frame Averaging Enter the number of frames you wish to acquire These frames are then averaged to reduce the noise level in your EBSP A higher number of frames will give cleaner EBSPs but will take longer to
341. nt Profiles and Show Candidate Elements are available here to assist you in confirming elements manually How to confirm elements Start with the largest peaks Press the question mark icon to select the Show Can didate Elements tool from the tool bar on the left hand side of the interface then double click on a peak in the spectrum viewer The candidate elements are dis played in a stacked spectra view on the right hand side of the window you can dou ble click on any of these elements to add or remove it from the confirm elements list Lead Pb Lal Double click to add or remove element You can control what overlays you see in the Spectrum viewer via the Confirm Ele ments Settings These overlays can be very useful in helping you to interrogate com plex spectra View Settings E Show Markers E Show Peak Shapes E Show Fitted Spectrum E Show Theoretical Spectrum E Show No Pulse Pile Up Correction 353 Press Include Exclude once you are satisfied with the identification of each element to build your list of the confirmed elements See Also Confirm Elements Settings on page 171 Confirm Elements Tools on page 174 Element Lists on page 191 Peak Labels on page 158 Compare Spectra amp MiniQuant Results on page 195 354 ON INSTRUMENTS The Business of Seience Calculate Composition Le Caloulate Composition EDS TEM In this step you can view quant results in
342. nts in Specimen Load from Profile Save to Profile Clear All Pm Sm Np Pu Am C Include b 4 Clear E Perform Auto ID During Acquisition Double click on the element symbols that you wish to include in the analysis All the included elements will be marked with the green color key in the periodic table To save the Pre Save to Profile i defined Elements in the current User Profile press It means when you load the User Profile next time these elements will be included in the analysis If you have already created a User Profile with the Pre defined Elements in the User Profile eee ee dialog press J Clear All Pressing will deselect the Pre defined Elements from the periodic table and they will not be included in the current analysis The peaks for the Pre defined Elements if included in the analysis are labeled in the Acquire Spectra step MiniQuant will display the quant results for these elements as Wt or a bar chart The Pre defined Elements will be marked as Pre defined in the Confirm Elements list box in the Confirm Elements Step There may be other elements in the Specimen which are identified by AutoID routine if the Perform AutoID during acquisition option has been checked in the User Profile dialog 311 Tip Right click on the Project or Specimen in the Data Tree and select Edit Notes to write or edit notes in any step of the Navigator See also Elem
343. nus Spectrum Viewer on page 321 Pulse Pile Up overlay in Confirm Elements step See the link below for details Confirm Elements Settings on page 171 a Pixel Binning available for Maps and Linescans this not only improves the image quality statistics on an image with low counts it also allows the large data sets to be processed more easily No need to decide the pixel resolution when processing data Overlay Mode i Binning 4 aps Benefits of binning are illustrated in the screen shot below With Binning maps are brighter have better statistics and more are detected by AutoLayer Without Binning maps are noisy and only a small number have sufficient amount of counts to be detected by AutoLayer See the link for details below How binning affects the quality of your data on page 373 Xill Compare step is now available in Guided Mode for ease of use a Variable spectrum acquisition termination Now the users have the ability to set their own termination criteria Acquisition Mode Counts Count Limit 00000 Pulse Pile Up Correction Candidate element list is now collapsible EBSD usability improvements and new functionality Solving Improvements Developments in indexing algorithms These changes make the indexing more robust so that it is easier to get good quality data The EBSD indexing algorithm It is less sensitive
344. o exclude this X ray line from the analysis In such a case it is recommended that you manually remove this X ray line from the sample model in the Setup Solver step and determine if the problem is soluble without this line When the analysis is repeated you should then find a better fit between the measured and predicted k ratios which will provide more confidence in your results Analysis Sample Summary This shows a summary of the model of your sample Note that the results are displayed in atomic fractions a Sensitivity The Sensitivity choice in the drop down box shows how variations in the beam cur rent can affect the analysis Also shown is how the uncertainty in the fixed quantities will affect the calculation of unknown quantities In terms of the sensitivity of the analysis with respect to small changes in beam current since the SEM beam current may change between the measurement of the Beam optimization standard and the measurement of the spectrum from the sample the k ratios will change in proportion The Sensitivity output shows how a change of 1 and 1 will affect each determined unknown Options Press the Options cog to open the Options window In this window deconvolution ele ments and standards files can be selected as well as thresholding of results and the window artefact correction a Deconvolution Elements You may select Deconvolution elements here in order to remove peaks aris
345. o compare results from one batch to another batch I am always looking for the same specified list of ele ments 83 You can specify the Element List for Quant from the three available options in the Quant Set tings dialog as shown in the screen shot below Element list Current Spectrum Select an Element list for the Fixed List e quantitative analysis from Fixed List and Current Spectrum the three options Iron Element Quant Line Fixed Weight Iron Titanium a Fe and Ti are selected as the Fixed List elements but you can overide the choice if required Add element Remove element Clear all elements Element List Quant Element List Details Current Spectrum This list includes the Pre defined Elements and elements identified by Auto ID and manually using the Candidate Element tool Fixed List You select the Fixed List option if you know what elements you wish to quantify Choose the elements from the drop down list as shown in the screen shot above Fixed List and Current Spectrum To quantify the elements in the above two lists select the Fixed List and Current Spectrum option MiniQuant results table will clearly display which list is being used A lock icon will be dis played against the Fixed List elements as shown in the screen shot below 84 EDS SEM Oy 45O ND INSTRUMENTS The Business af Science Sum Spectrum Compare In this example Fe a
346. o the Confirm Elements step in the Point amp ID package from the link below the Layered Image Viewer For details refer to Online Help See Also AutoLayer below Context Menu Map Viewer on the facing page How binning affects the quality of your data on page 373 AutoLayer By identifying and combining the elements that vary in a sample AutoLayer helps you vis ualize both phase and element distribution using a single image You can choose a color hue for each of the X ray maps and adjust brightness and contrast on each map individually or use the AutoBrightness or AutoGamma buttons to apply an automatic setting to all maps Colored maps can be mixed together or layered on top of an electron image to generate the Layered Image view and there is a control on each map win dow to select whether to include the map in the Layered Image combination The idea of mix ing is to make regions of different material content appear in different colors An overlay can be used to relate this material content to the topographic detail that is usually visible in the secondary electron image If the electron image is a backscattered electron BSE image the intensity may be controlled more by material content than by topography You may therefore prefer to assign a color to a BSE image and an option is provided on the electron image to either assign a color and mix it as if it was an X ray map or use a grey scale and overlay the mixture of colo
347. odel Note that it is a read only screen Analysis Lines 301 In the Analysis Lines tab you can view the analysis lines selected for quantification in the Con firm Analysis step It also gives you the details of the lines selected as part of the suggested analysis conditions in the Setup Solver step Note that this is a read only screen 302 The Business of Science EDS TEM Optimize 2 2 28 ccc ccc cece eee e cece eee eeeeeeeeceeeees 305 Calibrate aa0a0aa0a000 0000000000000000 0000000000000 306 Calibration Element 0022 22022 eee eee cece eee 308 Analyzer Guided 2 2 2 2 22 c cece cece cece cece ee eee eee ee eeee 309 Describe Specimen 2 222 222 2222 cece eee eee eeecceeceeees 310 Acquire Spectra 22 22 2220 cece cece cece ece cece cceeecees 313 Confirm Elements 22 02 2 22 e eee ee ceeecceeeeceeeeee 330 Calculate Composition 222 222 2 222 ee ee eee eee eee 332 Compare Spectra 2022 c eee eee ee eee eee eee eee 338 Analyzer Custom 2 22 0222 2 222 c eee eee ee ce eee cece eee eee ees 340 Acquire and Confirm 222 22 2 cece eee eee eee eeeeeee 341 Point amp ID Guided 2 222 22 cece cece cece eee ee eee 342 Describe Specimen 2 222 222 22e eee cece cece ecceeeeeees 343 6 a4 a tc 6 lt ae ae tnie ee ae eee 346 Acquire Spectra 2 22 22 eee e cece eee e cece cee ceeeeeees 350 Confirm E
348. oenen 370 How binning affects the quality of your data 373 362 EDS TEM Oy 45O ND INSTRUMENTS The Business af Science Acquire Map Data Acquire Map Data In this step you can acquire X ray maps from the full frame or selected regions of the spec imen The maps show the spatial distribution of all elements in the specimen The results can be displayed as a Layered Image where colors for each element are mixed together and over laid on the electron image or as individual maps Spectra from selected regions can be recon structed during or after data acquisition Generating a Layered Image or X ray maps can bea very useful way to find out what is going on in your specimen EXAMPLE I want to know where certain key elements are distributed over a defect Once I have this information I can determine what caused the defect and advise my production department How to Acquire and Manipulate Maps There are two different types of maps that you can acquire Window Integral Maps or Tru Maps Historically Window Integral Maps have been the standard mode for X ray maps These are ideal when there are no overlapping peaks and you are not looking for trace elements in your specimen The second mode of mapping is with TruMaps which are ideal for specimen containing ele ments with overlapping peaks and removes false variations due to X ray background You can easily switch between t
349. ofile ae e ee ee ee 5 Pe Nb No Te c h Save the Predefined Elements to the User Check this box to Profile enable AutoID during the spectrum Pm m Eu acquisition Np Pu Am Include z E Perform Auto ID Dunng Acquisition Note that the Pre defined Elements are saved with the current Specimen Changing the Predefined Elements will only update the Pre defined Elements in the current Specimen It will not update any existing Specimens in the Project Data View Current Site Data Tree z Project 1 Specimen 1 Specimen 2 4 Site Electron Image 2 Spectrum 9 Spectrum 10 Spectrum 11 a r aS T gt g 4 lt Site3 Electron Image 3 Spectrum 1 Spectrum 13 Spectrum 14 82 Oy AE ED EDS SEM INSTRUMENTS The Business of Science The current specimen is the one that you are presently analyzing processing the data from For example in the screen shot above Specimen 3 is the current specimen Spec imens 1 and 2 are the other specimens in the Project Identified Elements The Identified Elements will include a Any Pre defined Elements Elements identified by Auto ID a Any additional Elements identified manually If the Pre defined Elements have been specified these will be included for identifying and labeling peaks in the current spectrum automatically Note that the Identified Elements are saved in the Spectrum Perform Auto ID During Acquisi
350. ol This section appears only if a forward scatter detector is correctly configured To control set tings for the signals from the forward scatter detection diodes click the Settings button to open another dialog If you select the Auto checkbox before you start a new FSD acquisition the software auto matically adjusts the signal from each diode for optimal brightness and contrast The opti mized electron image then appears after a delay of a few seconds When you first start the software the Auto check box is already selected for you See Also AutoLock on page 133 Scan Image on page 418 Scan Image Toolbar The Toolbar is located near the top left side of the Scan Image window Tools are provided to manipulate and annotate the image Pan and Zoom You can move the image using the Pan tool Use the wheel mouse to zoom in and out Annotation There are five different tools to add annotations on the current image as shown in the screen shot below 424 EBSD To edit an annotation double click on it to select it the editing handles will be displayed Use the handles to edit the annotation To delete an annotation select it by double clicking on it and then press the Delete key on the keyboard To delete all annotations on an image choose Select All from the Annotations context menu on the image viewer and then press the Delete key on the keyboard Information Select the Show Data Values tool from the tool
351. ol from the toolbar and then click on the image to start mon itoring as you hold down the mouse From the Spectrum With this tool you can view the Energy keV and counts in any channel of the spectrum Simply select the Show Data Values tool from the toolbar and then hover on spectrum The values will be dis played as you move from channel to channel From the Electron Image Clicking anywhere on the image will display the Intensity value at that pixel position Monitoring the signals Click on the acquisition tool and press the mouse down on the electron image to see the monitoring signals for both EDS and EBSD Move the mouse over the image to monitor both the EDS and EBSD signals Once the mouse is released acquisition will take place accord ing to the acquisition settings for EDS and EBSD Spectrum Monitor provides a dynamic way to see what X rays are being detected at any given moment It is useful for a quick survey of the specimen to find an area of interest for analysis Soectrum Monitor uses the current spectrum acquisition settings with the addi tional setting of the refresh rate for monitoring the spectrum This refresh time is referred to as the Buffer Size The default is 20 but can be changed under the Settings for Soectrum Mon itor in the Miniview Increasing the Buffer Size corresponds to a longer refresh rate Data collection 475 Click on the acquisition tool nin and click on a location on the electron
352. olbar and other nearby controls The acquisition toolbar above the electron image and below the Navigator has buttons for starting and stopping the image acquisition the Settings cog for selecting the image acqui sition parameters and a button to link unlink images for manipulation F New Site Scan Image E START STOP Settings Select Second Image None 3 418 The Business of Science Control FSD only EBSD Description Displays up to three combinations of mixed image and individual images Your selections are retained in your user profile Click to start the image acquisition according to the cur rent acquisition parameters Click to stop image acquisition Acquisition stops at the end of the current frame Click again to stop imme diately If you navigate away from the step acquisition stops at the end of the current frame To change the acquisition parameters click the Settings cog on the Acquisition Toolbar to display a dialog You can select Image Scan Size Dwell Time us Input Signal the labels here reflect whatever was set during the installation for example SE BSE or FSD either Con tinuous Scan or Number of Frames and Frame Time secs If your specimen is drifting you can activate AutoLock to ensure that any analysis corresponds to the true loca tion on your image 419 Control Description Mixing Mode Combines signals from the diodes to form a mixed image
353. ols are above and below the phase maps Settings Description Displays the phase image or the phase maps or both Sets the number of maps per row in the Standard and Interactive displays 232 OX sO EDS SEM INSTRUMENTS The Business of Science Settings Description Offers a choice of map display Standard you can add individual images or remove them from the combined image Interactive similar to Standard Links the zoom and pan of all the maps Summary a compact display where you can change the color of each phase Links images for manipulation of all layers using the Pan or Zoom controls Changes the brightness and contrast of the cur rently selected image or map Adds the selected phase map or electron image to the combined phase image Minimizes a map The Minimize icon is in the top right hand corner of each map This is useful if you have too many maps in view The map moves to the Minimized Phases tab below the displayed maps Removes a map or electron image from the phase analysis This icon is in the top right hand corner of the image Restores a minimized map to its normal size The minimized maps are on the tab below the dis played maps This icon is in the top right hand corner of each map Sets the color of the phase The list is available only in the Interactive and Summary map display See Also Analyze Phases on page 375 Processing toolbar
354. on The Standardization file with ois extension and User Pro file file with config extension are exported You can share these files with other users using the Import option in the User Pro file dialog 269 LayerProbe The LayerProbe navigator has the following steps 2 0 LayerProbe 00 0o cone otnca telus dtet Seb cing lt tdc los aooaa 271 Describe Specimen _ 2 222 022 cee cece c cece cece ce cece ee cceeeeeees 273 Describe Model 22 222 2 2 cece cece cece cece cece eeeeeeee 276 Scan Image 250k ooo dee east een Satna soul cst ene a guess 280 PECGUITE SDECE a sis Spe satcteodae eng tei darea i dee deda aaah 284 Confirm Analysis 22 20 22222 c cece cece eee ec ccc cee eee cceeeeees 287 Calculate Layers nce tub sai een ese ea eee eduieauss 292 Edit Materials 2 000000000 000000000000000 000000000000000 eends ees 294 Simulate Spectra 00000000000000 000000 0000000000000000 cece eeecceeeeeees 296 Set Up Solver 2 0 0 0 oleic 0000000000000000 ec ceeecceeeeeees 299 LayerProbe Settings 0 0 222 c cece cece eee eee cece ee eee eee eee 301 Da O RD FT LayerProbe INSTRUMENTS The Business of Science LayerProbe cc cccccseesseeesteneee Introduction LayerProbe is designed to calculate the thicknesses and compositions of multilayer structures on a substrate The program contains tools which enable you to determine the optimum con ditions kV beam current li
355. on conditions You will need to fill in the acquisition conditions when loading the EBSP in order for the software to be able to analyze the EBSP Depending on the calibration information available with the EBSP the calibration conditions will either be those based on the system calibration or a previously acquired calibration file In the latter case you will need to add additional information into the required fields Settings 444 EBSD The Business of Science Under Settings adjust the Hough resolution number of bands and band detection method to ensure you aid the identification of the acquired EBSP You should also ensure that you have included the phases you wish to use and their corresponding number of reflectors Band Detection Area a Selecting the Edit Band Detection Area tool on the Optimize Solver toolbar will allow adjust ment of the band detection area When the tool is active the Area of Interest will be displayed on the EBSP and by use of the mouse the area can be moved or resized Edit EBSD Bands The application will automatically detect a number of Kikuchi bands depending on the number of bands you have set it to detect However you have the ability to edit any existing band delete bands or manually add bands In order to interact with the detected bands select the Edit EBSD Bands tool on the Optimize Solver toolbar This will allow you to delete bands draw new bands or modify existing bands
356. on above the map BEDS Data display Standard Window Integral maps counts in the energy window are acquired for the element list chosen Ti Kal for analysis These are raw X ray maps Cr Kal which are not corrected for back Mn Kal ground or peak overlaps Map Sum Spectrum Mg Kal _2 a r EDS Layered Image 2 Second mode of mapping is TruMap You can process the map data as Tru Maps which are corrected for back ground and peak overlaps Mineral im ported image EDS Layered Image It is a composite image generated by overlaying selected X ray maps on top of the electron image Viewing and Manipulating Maps You can choose how you wish to view your data Various tools are available to manipulate and view the X ray maps Map Size You can choose the number of maps per row using the slider bar for displaying maps you wish to view in the Standard and Interactive display mode EDE L Display Modes 366 EDS TEM Oy 45O ND INSTRUMENTS The Business of Science Maps can be viewed in three different display modes available from the drop down list on the Display toolbar Standard Interactive In the Interactive mode you can change the color of individual maps from the Hue drop down list The Layer Mode can also be chosen from Mix and Overlay modes available from the electron image Summary In the Summary view you see details of the energy window and X ray lin
357. on page 424 Scan Image Settings on page 421 FSD diode controls on page 432 Context Menus Image Viewer on page 157 Export Settings on page 132 AutoLock on page 133 349 Acquire Spectra A Acquire spectra In this step you acquire spectra from the current electron image SE BSE You can also recon struct spectra from a Layered Image or X ray map if you have already acquired SmartMaps Real time Compare and instant MiniQuant options are also available here You can display the components that you are working on such as image and spectrum using Eliz ee the controls on this toolbar located in the top right side of the screen You have choice of displaying image and spectrum as shown in the screen shot below or just an image or a spectrum full screen File vew Tehni Tone Help r 9 o Fae i ly Teriba s I zarg r 7 me he feed eT pity k Fene Looe Spectr F START STOF jeie 3 Saecttecorndinmage home SE Electron Image 1 Sprcir tries _ Wit 16 80 rem Inpart Rrte Sie Arps Citar Rather SGA ope Dead Time 25 Penna Tirran 350 EDS TEM 45O ND INSTRUMENTS The Business af Science There is an acquisition toolbar near the top of the workspace Acquire Spectrum gt START STOP settings SelectSecond mage None E E It has controls for starting and stopping the spectrum acquisition There is a Settings cog for selecting the acquisition parameters F
358. on will be available during live map acquisition and reanalysis Simply select Stored or Live in the toolbar to switch between live monitoring and stored mode Stored pattern mode will be used when you are doing your offline reanalysis For live orientation you will need to specify in settings how often you would like to refresh the rate of the orientation values Phase Fraction The phase fraction percentage indicates how many pixels have been indexed to a particular phase in your specimen The percentages of the phases and zero solutions are displayed and each will have a color fraction percentage and total pixel area count Full map and region statistics are available now to compare results These absolute numbers will change after noise reduction in the post processing software Tango because zero solu tions will likely be replaced by neighboring phases Reanalysis Introduction 465 Data reanalysis allows the reanalysis of a map region with different acquisition settings i e phase Hough number of bands and number of reflectors It also allows you to add and or remove phases in case you may not know all the crystallographic phases present or different regions on the specimen require reanalysis with different phase lists In addition it is possible to reanalyze data multiple times in order to standardize acquisition settings for specific spec imens or until When reanalysis of map data containing both EDS and EBSD data is per
359. oncentrations that are being determined For example you may find out that provided a contamination layer is less than a certain thickness it will have no serious effect on the accuracy of the results Again this can be investigated using the simulation tool to syn thesize realistic spectra that can be analyzed without wasting time on the microscope The general principle is that the more precisely the problem can be defined the better chance that LayerProbe will be able to solve it and the more precise the results will be for a certain measurement time When you tell LayerProbe the approximate values of layer thick ness that is to be determined the Calculate Solubility tool will try to anticipate all possible values when working out if the problem is solvable When you are ready to do a real analysis on the microscope the system will allow acquisition of spectra and will also optimize the accuracy of the quantitative measurements Data is then saved in a project and spectra then analyzed using the LayerProbe software The results will show the sample description the determined values for the unknown thicknesses and con centrations and the calculated precision in these results As previously described the sen sitivity analysis will show how any guesses in the fixed values would affect the results and also shows how a small variation in beam current during the experiment would affect the results 272 LayerProbe O 45O ND INSTRUM
360. onfirm Elements _ 2 2 222 022 e ee eee eee cece cece eee ceeeeceeseeeeeees 170 Calculate Composition 2 222 222 2 22 ec eee cece cece eee ceeeeeees 185 sae Ox FO RD EDS SEM INSTRUMENTS The Business of Science Scan Image x Scan Image In the Scan Image step you can acquire an electron image into a Site A Site is like a folder which contains images and analyses for a particular area on a specimen For EDS if you do not want to collect an image and just want to acquire spectra you can skip this step and go straight to the Acquire Spectra step You can have any number of images in a site Just ensure that the images you want to keep are padlocked in the data tree to stop them being overwritten as shown in the screen shot below Data View Current Site Data Tree Hedronimagel SSO You can toggle between saving or replacing the current image with successive image acqui sition If your specimen is drifting click the Settings cog and activate AutoLock The Scan Image step has several tools for manipulating and enhancing electron images The acquisition toolbar above the electron image and other nearby controls Scan Image toolbar a vertical toolbar on the left for manipulating and annotating the image Ifa forward scatter electron detector FSD is fitted extra controls are available for combining the signals from each diode into a mixed image Acq
361. oodness of fit parameter How ever it is independent of the band detection process and larger AFI values indicate better solutions The AFI value is also affected by the quality of EBSP Orientation These are the three Euler angles that describe the orientation of the crystal lattice as deter mined by the indexing procedure Refinement P The refinement routine tries to compensate for any instability in the readout of WD or ID You may choose to refine your calibration based on a selected solution You should ensure that this solution is correct as this refinement will potentially produce an offset in Working Dis tance WD and Insertion Distance ID that will subsequently be applied when indexing any subsequent patterns Phases for Acquisition 446 EBSD The Business of Science You should ensure that you have included phases you wish to solve with within the Phases for Acquisition area If you wish to add or delete any phases this can be done in the Describe Specimen Step However you can include or exclude individual phases from the list within the Optimize Solver step or change the number of reflectors and color can be set per Phase in this step In addition details about any highlighted phase can be viewed in the Phase area by selecting the 3D Phase View Phase Details and Reflectors tabs See Also Optimize Solver Settings below Context Menus Image Viewer on page 157 Brightness Contrast and Gamma Contro
362. oothing applied 3 Data averaged over three points 5 Data averaged over five points As an alternative way to reduce the effects of noise in the linescans you can apply a binning factor Binning is particularly effective when using TruLine See Also How binning affects the quality of your data on page 373 398 Mg Kal_2 ii PT ri Ct igi i ral a 180 210 240 2 0 300 a 30 Linn Smoot EDS TEM Oy 45O ND INSTRUMENTS The Business of Science Linescan Data The data tree contains a Line item under the Site this is the container for the line data By default this is labeled as Line Data where is an auto increasing number under the cur rent site Site 1 as shown below Project 1 ig Specimen 1 4 Sitel _ Electron Image 1 Line Data 1 Line Data 2 Line Data 3 y CA mora Line Sum Spectrum Mg Kal_ Ti K l Cr Kal Mn Kal Fe Kal Br Lol 2 The Line item is the container for EDS Data All linescans and the sum spectrum are contained within the EDS Data container For details right click the icon Taa The sum spectrum is called Line Sum Spectrum OS AN The name of the element linescan Line TruLine or QuantLine is composed of the element sym bol and the line A spectrum extracted from a single point on the linescan See Also Data Tree on page 85 399 Exporting the linescan data Right click on the linescan viewer to access the Export menu It has sev
363. or channel images Select this mode if you are inter ested in seeing density atomic Z contrast signal FSD Topo Orientation uses lower FSD detector chan nel images Select this mode if you are interested in seeing orientation contrast signal Custom include and exclude FSD detector channel images of your choice When you select either of the first two modes the soft ware automatically uses the FSD diode channels asso ciated with that mode For example FSD Z mixing mode uses the upper and side FSD diode channels The FSD Topo Orientation mixing mode always uses the lower FSD diode channels Custom mode allows you to mix any FSD diode channels Select Second Image Selects further images to compare with the electron images for example a forward scattered electron image This control is available only when the map dis play is for an image only Fm sz C Sets the number of images per row in the Standard and Interactive displays FSD only Offers a choice of image display ESD onl Standard you can add individual images or remove omy them from the mixed image Interactive similar to Standard You can also change the weighting and color contributed by each image Summary similar to Interactive and in a more com pact display Er Links images You can simultaneously manipulate all the layers using the pan or zoom controls 282 LayerProbe The Business of Science Control Description
364. or details see Acquire Spectra Settings link below The toolbar located on the left side of the workspace has various tools for image and spec trum manipulation enhancement annotation and area selection For details see Acquire Spectra Toolbar topic from the link below There are manual and auto brightness contrast and color controls available for the image view You can use these controls to enhance and high light certain features in the image The Compare Spectra amp MiniQuant Results option is available in the top right corner of the Spectrum viewer You can compare the current spectrum with any other spectrum from an opened Project on the Data Tree Instant MiniQuant results can be viewed in a table or a bar chart See also How to acquire spectra on page 148 Modes of X ray spectrum acquisition on page 150 Acquire Spectra Toolbar on page 151 Acquire Spectra Settings on page 313 Context Menus Spectrum Viewer on page 321 Export Settings on page 132 Peak Labels on page 158 Element Lists on page 191 3391 352 EDS TEM Oy 45O ND INSTRUMENTS The Business of Science Confirm Elements ontinm Elements This step has been designed to help you confirm the elements that have been identified by AutolID in your spectrum These elements are then used to create a confirmed elements list for qualitative and quantitative analyses Extensive tools including Element Series Markers Overlays Eleme
365. ou have included in the Phase Search lists This may take a few seconds if you have many potential phases Note that solving does not involve the Phases for Acquisition list in Describe Specimen When the indexing process is complete any solutions will be displayed below the EBSP in the Analysis area If there is more than one solution scroll through the different solutions and vis ually check the accuracy of the indexing by viewing the simulations The MAD value displayed in the solution list will provide a good estimate of how well the simulation matches the EBSP Whilst higher MAD values indicate a better match it might not be correct if the wrong phase or settings have been used in the process so always check that the solution matches the EBSP Select the solution from either the phase list or solution list Multiple Solutions In an ideal situation there will be one solution which is clearly correct However there may be several different phases which appear to give a good match In such cases one or more of the following steps may help to identify the correct solution a Check the simulation using more reflectors by adjusting the number of reflectors in the Phase Search results view Adjust the database search by adjusting the compositional ranges for individual ele ments if necessary previous step Optimize the band detection by manually adding more bands if necessary 481 a Switch on Advanced Fit Note that if
366. own in the screen shot below Specmen Geometry Pre defined Elements Press this to load a profile 4 for your Toad from Profile analysis Predefine your elements from the Periodic table Click on an element first to select it and then press the Include button Save to Profile Na Mg en a a ee a i u S Rb Sr Y Zr Nb Mo Tc Ru re Save the Predefined Elements to the User Check this box to Profile enable AutoID during the spectrum Pm acquisition Np Include h E Perform Auto ID During Acquisition 191 Note that the Pre defined Elements are saved with the current Specimen Changing the Predefined Elements will only update the Pre defined Elements in the current Specimen It will not update any existing Specimens in the Project Data View Current Site Data Tree ad Project 1 Pa Specimen 1 d g Specimen 2 4 gt Site Electron Image 2 Spectrum 9 Spectrum 10 Spectrum 11 C 4 gt Site3 Electron Image 3 Spectrum 12 Spectrum 13 Spectrum 14 The current specimen is the one that you are presently analyzing processing the data from For example in the screen shot above Specimen 3 is the current specimen Spec imens 1 and 2 are the other specimens in the Project Identified Elements The Identified Elements will include a Any Pre defined Elements Elements identified by Auto ID a Any additional Elements identified manually If the Pre defined Elements have
367. page 353 Calculate Composition on page 185 User Profile on page 22 Compare Spectra amp MiniQuant Results Real time Compare and instant MiniQuant options are available in the Acquire Spectra Con firm Elements and Calculate Composition Comparison of Results Two Spectra template steps User can see results without having to move away from the acquisition mode Using these options you can See your results during analysis Compare your current spectrum to a control spectrum during acquisition a View MiniQuant results in a table or a bar chart Mii L r i Click S in the top right corner of the Spectrum Viewer in Acquire Spectra Confirm Ele ments or the Calculate Composition window to access the Compare amp MiniQuant options 180 EDS SEM OXF INSTRUMENTS The Business af Science e In the above example Spectrum 1 is the current spectrum and Spectrum 2 is the comparison spectrum You can select the comparison spectrum from a Project currently available in the Data Tree It can be from any Project any Specimen and any Site of Interest currently available in the Data tree To choose the comparison spectrum click on the down arrow Spectrum 2 in the above example Spectra available in the current Project Specimen and Site of Interest are displayed as below Proect1 Speamenil Click on the spectrum in the display to select it for comparison The selected spectrum will be overlaid as
368. pe parameters can not be read automatically you will need to manually enter the values of kV and magnification directly into the spaces provided in the Microscope Control Access the Microscope Control by pressing located on the right hand side of the Status Bar All images subsequently collected will be acquired with these parameters Note that if you change the magnification on the microscope and forget to enter this new value into the Magnification box in the Microscope Control window the scale marker will be incorrectly calculated Accelerating voltage kV What is it The voltage applied to the electron gun that causes electrons to accelerate down the elec tron optic column The higher the accelerating voltage the greater the energy and the shorter the wavelength of the electrons striking the specimen Why is it important The energy of electrons striking the specimen dictates what X ray lines can be excited and their relative intensities For quantitative calculations the software needs to have an accurate value for kV At higher kV the higher energy incident electrons penetrate deeper and scatter more widely into the specimen so the excitation volume for X rays is larger What value should I use Choosing 20kV is a good starting point particularly if the specimen is unknown At this kV at least one series of X rays from every element will be excited Choose a lower kV if you are concerned about Accuracy of
369. phase fraction while col lecting See Construct Maps on page 463 Improvements in image acquisition for forescatter detectors Collect up to 6 individual FSD images simultaneously The number of images collected depends on the number of independent diodes on the detector Functions include 6 channel FSD images and a mixed FSD image are acquired and viewed in one inter face Automatic optimization of each channel before scanning Offset and gain of each channel can be adjusted manually during image acquisition The weight of signal intensity for each channel in the mixed image is set to get the best image Color may be selected for each channel image a Optimization is possible on a reduced area by selecting a reduced area map and the optimization factor applied to the whole map This is useful for images where very dark regions such as a hole or very bright regions can distort the image opti mization See Scan Image on page 418 Drift correction using FSD images as references V What s New in AZtec 2 1 OXF INSTRUMENTS The Business of Science A new option allows the use of the FSD image as the tracking image to monitor and correct for drift On a tilted sample the FSD image often offers the best image for monitoring drift because it can show more detail than the secondary electron image or backscattered electron image See AutoLock Settings on page 138 Export Raw Unprocessed EBSPs fo
370. play Layer modes on electron images can be useful for showing topographical and compositional detail in a layered image Both layer modes add the color components for each map together at each pixel In Overlay mode the brightness of each pixel is determined by the electron image The color is determined by the composite red green and blue of all the other images This mode shows more clearly the relative changes in intensity between the maps In Mix mode the color is determined by the composite red green and blue of all the images including the electron image This mode tends to make variations in the absolute intensities of the maps more visible At the Acquire Map Data step select Interactive from the drop down list above the maps and images You can then choose a layer mode from a drop down list on the electron image By default the layered image for the electron image is in Overlay mode This is ideal for view ing the overall chemical distribution of elements on a specimen image See the next example which shows the selected maps and the layered image The next example uses the same area and adds the backscatter electron BSE image in Mix mode The addition of the compositional information in the BSE image to the topographical information in the SE image gives better definition to the overall layered image 216 EDS SEM OSs INSTRUMENTS The Business of Science 10m To overlay the den
371. played in a stacked spectra view on the right hand side of the window you can dou ble click on any of these elements to add or remove it from the confirm elements list Lead Pb Lal Double click to add or remove element You can control what overlays you see in the Spectrum viewer via the Confirm Ele ments Settings These overlays can be very useful in helping you to interrogate com plex spectra View Settings E Show Markers E Show Peak Shapes E Show Fitted Spectrum E Show Theoretical Spectrum E Show No Pulse Pile Up Correction 115 Press Include Exclude once you are satisfied with the identification of each element to build your list of the confirmed elements See Also Confirm Elements Settings on page 171 Confirm Elements Tools on page 174 Element Lists on page 191 Peak Labels on page 158 Compare Spectra amp MiniQuant Results on page 195 116 EDS SEM ON INSTRUMENTS The Business of Science Calculate Composition amp Calculate Composition In this step you can view quant results in more detail using any of the Available Templates To view result select the template that you wish to use Available Templates Quant Result Details summary Table Single Spectrum Label Line Sum Spectrum eee aree pa gada Element List Type Current Spectrum summary Table Multiple Spectra Processing Option All Elements Full Results Table customizable Singl
372. ponents Scan Image Acquire Line Data and Construct Linescans are laid out as separate steps in the Guided mode of the Linescan application These three components are combined in the Custom mode to give you a single workspace called Acquire and Con struct It provides the convenience of working in one screen without having to move away from it The user interface components are docked in the four quadrants in the workspace Each com ponent can be undocked as a free floating window It can be dragged on to another monitor resized or displayed in the full screen view There is a toolbar located near the top right corner of the workspace with icons which allows you to toggle on off each component The user interface elements are described below Acquiring an electron image and line data In the top left quadrant you can acquire an electron image first and then define a line to acquire the line data E E gt START 1 Press to select the image acquisition mode Then press to start electron image acquisition 2 On completion of image acquisition press to switch to the line data acqui sition mode 3 Press aS to select the line tool in the toolbar on the left 4 Click on the image to set the start point and then drag the mouse to define the line Release the mouse to set the end point A line with start and end points is defined on the image START 5 Press to start the line data acquisition A relevant section
373. proc essing z Shows the progress of the proc essing For more details hover the cursor over the progress bar for a few seconds Cancel Processing Stops the processing Adjusts the settings used dur ing the processing Boundary Tolerance con trols the behavior at the boundaries of each phase The Grouping Level deter mines the numbers of phases that you see See Also 384 EDS TEM Oy A5O ND INSTRUMENTS The Business of Science Analyze Phases on page 375 Analyze Phases settings on page 381 Finding phases on page 376 Toolbar for Phase Map These controls are at the top left side of the window ra Moves the image Click the Pan tool then click and drag the image Use the mouse wheel to Zoom in and out Normalizes the spectra Adds annotations to the current image The tools include Caliper Angle Text Rectangle and Ellipse Defines points and regions on a map image to extract spectra Shows the energy and counts at any point in the spectrum viewer in the bottom left corner Shows the phase at any point in the phase maps in the top right corner See Also Analyze Phases on page 375 385 Map Custom In the Custom mode the Map navigator has two steps The Describe Specimen step is covered in the earlier section The step which is unique to this navigator is described here Acquire and Construct 2 222 222 ee cece cee eee ee eee
374. processing the spec tral data If you wish to deconvolve elements from a spectrum select the required element from the drop down list and press Add element Further elements can be added or removed using Add element or Remove element respectively e Threshold Quantitative Results To enable Threshold Quantitative Results check this option in the Quant Setup tab If thresholding is enabled any X ray line whose k ratio value is below the minimum value allowed by the Stratagem engine Is assigned the minimum allowed k ratio value in order for the calculation to proceed without an error message e Correct for window artefacts To enable Correct for window artefacts check this option in the Quant Setup tab Checking this option ensures that the contribution to the spectral peaks from the detector window material is removed prior to quantification of the spectrum e Quantitative Standardizations The system is supplied with factory standardizations To use your own standards for quan titative analysis you first need to acquire spectra from standards and perform at least one standardization using the Standardize step on the Optimize navigator When you have done this your user file will be available to select under Quant standardizations in the EDS Lay erProbe settings If the Factory button is selected only Factory standardizations can be used for the calculation of quantitative results Model In the Model tab you can view the m
375. ps Selects how layers are selected in the layered image Manual you select the X ray maps to include in the layered image Automatic the software chooses maps with the max imum intensity up to the number that you type here Filters out some noise by applying a smoothing level If there is not enough data the maps might con tain alot of noise which masks the distribution of the elements This operation applies a low pass filter to an image to smooth the data The smoothing level low pass filter uses the following 3x3 kernel 1 9 1 9 1 9 Ib SAWS VAS V9 T919 The smoothing level low pass filter uses the following 5x5 kernel 1 25 1 25 1 25 1 25 1 25 1 25 1 25 1 25 1 25 1 25 1 25 1 25 1 25 1 25 1 25 461 ACB while acquiring Applies automatic brightness or auto matic gamma to maps during acqui sition depending on your previous selection of Auto Brightness or Auto Gamma 462 EBSD OXF INSTRUMENTS The Business of Science Construct Maps Construct Maps In this step you work more closely with your acquired maps and construct new EBSD and lay ered images If you have acquired an EBSD map with stored EBSPs you can also reanalyze a map region with new settings such as new solver settings or by including different phases This step displays a layered image maps and electron images You can choose how to view your data and you can add or remove maps to build the laye
376. r cross correlation applications Raw 12 bit patterns as collected from the camera can be stored as TIFF files These patterns are not corrected for background magnetic field or lens distortion These patterns are pre ferred for cross correlation applications such as CrossCourt Unprocessed EBSPs are created during acquisition and collected in a folder with a selected local destination Image format is uncompressed TIFF Ifrequired the processed EBSPs can also be saved See Acquire Map Data Settings on page 457 General performance and other EBSD improvements a Monitoring function for extract tool in Phase ID and Optimize Solver AutoID of the peaks in Spectrum Monitor in Phase ID and in the Mini View Easy identification of the elements in the sample The phase key in the phase map lists only those phases found in the map Some improvements to naming consistency so that the name of EBSD Detail dialog box is constant with the acquired map See Identify Phase on page 480 Optimize Solver on page 444 Acquire Map Data on page 450 and Construct Maps on page 463 General improvements Report Template Generator a Licensing improvements AZtec and INCA a Network Licensing AZtec and INCA Interface modifications and GUI usability improvements Report Template Generator In addition to the comprehensive report templates available for reporting a Report Tem plate Generator now allows the design of p
377. r or Point amp ID where you have setup your acquisition parameters to optimize your quantitative analysis If you now wish to acquire SmartMap data and you think you may wish to recon struct spectra from your SmartMap data and then quantify these spectra you should maintain these acquisition parameters This means that you may have to acquire data with along Process Time to maximize resolution but limit the maximum acquisition rate 2 You may have been working in either Analyzer or Point amp ID and you want to view the distribution of elements whose main peaks do not overlap as a map or a lines can In this case you should use a shorter Process Time which will mean that you can work with higher acquisition rates and shorter acquisition times The choice of Proc ess Time will very much depend on your sample and what you wish to do with your SmartMap data once it has been acquired 3 If you have started your Project in Map and you are analyzing an unknown sample we recommend that you use a long Process Time in order that you do not miss any detail in your spectrum However if you only wish to map certain elements whose 98 EDS SEM ON INSTRUMENTS The Business of Science main lines do not overlap you can afford to shorten the Process Time and increase the acquisition rate by increasing the beam current Acquisition Mode There are three options to terminate the acquisition Auto Live Time and Counts If Auto mode is s
378. r to the next layer etc Templates that show results for multiple spectra include a statistics table that shows Max Min Average and Standard Deviation for each visible results column in the main table Additional notes 2292 LayerProbe Oy 45O ND INSTRUMENTS The Business of Science All templates that display Quantitative results include an Unknowns Only check box which is un checked by default You can check this box to exclude all Fixed thick nesses and concentrations from the results and statistics tables Ifyou wish to change which standardization file or deconvolution elements to use press the Options button to display the LayerProbe Options window Press the Requantify button to display the recalculated results 2293 5 Edit Materials In this step you can build a database of materials that can be used to populate layers within a model The composition and density of commonly used materials can be stored here so that they do not have to be re entered every time How to add an entry to the Database 1 Enter the name of the material in the Name text box 2 Choose a composition type from the two available options Number of Atoms or Weight Select Number of Atoms if you know the chemical formula e g for alu minum oxide enter Al203 in the Composition text box The elements and their Atomic and Weight are populated automatically in the table 3 Enter the Density g cm i
379. rawn on either side of this point The spectra in the Compare viewer are scaled to the average value of cps eV Y axis in the window Normalize Spectra Region e Select this option from the toolbar near the top left of the Compare Spectra screen e Click and drag to set a normalization region along the X axis e The spectra in the Compare viewer are scaled to the average value of cps eV Y axis in the normalization region selected in the previous step Smooth The Smooth function is available from the context menus of the spectrum viewer This is use ful when comparing spectra where small differences may be obscured by statistical scatter The smooth function applies an energy dependent filter to the spectrum This has the effect of slightly broadening the peaks and also filtering out the rapid fluctuations due to statistics Statistical fluctuations can sometimes appear like a real peak When it is difficult to decide whether a peak is present or not the smooth function substantially reduces the statistical fluctuation so that any real peak becomes more visible 3905 Point amp ID Custom Point amp ID is an image centric application that requires the acquisition of an electron image prior to X ray spectra acquisition There are two modes of operation Guided and Custom In the Custom mode the Point amp ID navigator has three steps Describe Specimen and Compare Spectra are described in the earlier sections The new step
380. re used to find the edges or centers of bands during automatic band detection Depending on the number of bands you have entered under Settings these maxima will be marked with numbers to show which ones correspond to the detected bands The highest number cor responds to the strongest peak You may toggle between the two icons on the Hough Space display window to switch between showing all bands or currently selected band Move the mouse over Hough Space and the corresponding location on your EBSP will be dis played Hover over the maxima to see how it relates to the band in the EBSP Solutions This area shows the results of the EBSP indexing process A simulation of the selected solu tion will be overlaid on the EBSP allowing a visual comparison between the simulation and the original EBSP Note that the order of the solutions can be changed if you select Use Band Widths in Sorting under Settings in the Processed EBSP area if you are using the edges of the bands during band detection See later The following parameters are displayed for each solution MAD MAD or Mean Angular Deviation is the goodness of fit of the solution The smaller the number the better the match between the detected Kikuchi bands and the simulation A number less than 1 is acceptable for most systems If Advanced Fit has been switched on then the Advanced Fit index AFI will also be dis played instead of the MAD This like the MAD value is also a g
381. recision is not good enough you can increase the acquisition time or count rate and try again All this can Zi Ls be done very quickly without having to waste any time on the microscope before it is known that the method will work Sometimes the best conditions will fail and this will usually be because there are too many unknowns or because the kV range is not extensive enough The way around this is not to ask for so many unknowns In many problems there are certain concentrations or thick nesses that are critical and others that are not important For example there might be a layer of contamination present but is not what the experiment is setting out to measure By mak ing these unimportant variables fixed rather than unknown a previously unsolvable problem may now be solvable When a problem is unsolvable the best conditions tool will sometimes be able to advise which unknown variables are making the problem unsolvable and fixing one or more of these will often work Of course making a thickness or composition fixed means having to estimate the value rather than determine it LayerProbe allows you to make a guess at the value The obvious question is does it matter how good my guesses are and this depends on the exact details of the problem However there is another tool available called Sensitivity analysis and that will show just how the uncertainty in the guesses will affect the values of the critical thick nesses and c
382. red Image icon in the top left hand corner of each map If you have lots of maps it may be useful to minimize some of them pressing the minimize icon 2 in the top right hand corner of each map You may want to delete a map from the analysis completely In which case press the delete icon Ei in the top right hand corner of each map This means this element will not be identified automatically AutoID and will be excluded from the current analysis Note If an element is present in a specimen deleting or excluding it will affect the TruMap results EDS TEM The Business af Science Inthe map display settings you can sort maps alphabetically by atomic number or by maximum map intensity You can also smooth maps by choosing the smoothing level from the Settings Using the Auto Brightness and Gamma buttons on the bottom right hand corner of the Map display window allows you to change the Bright ness Contrast and Gamma for all the maps The Auto Brightness button optimizes the maps to give the best Layered Image and the Auto Gamma enables you to see all the map data including background noise You can choose the color for your maps adjust intensities and decide which maps to add to the Layered image Alternatively you can let the software do this auto matically Pressing the AutoLayer button which is located in the bottom right hand corner of the Map Display window will automatically scale and color all
383. red X ray maps If you choose different colors for similar maps and mix them together the resulting mixture color will not bear any relationship to the original colors so it will be difficult to make sense of the layered image If you are analyzing specimens where you know what elements are likely to appear then manual color mixing is straightforward However for more complex situations or when you are dealing with an unknown specimen you should find the AutoLayer function helpful If you have a series of X ray maps displayed the AutoLayer button will run an algorithm to analyze the spatial content in the maps to decide and select the best maps to use for the lay ered image It will also adjust contrast and brightness and assign a suitable color hue to the maps to give a useful layered image If maps have a lot of statistical noise they are unlikely to be selected otherwise the layered image would show a lot of random colored dots When a set of maps show similar spatial content they will be assigned the same hue but only the best map will be chosen for the mix Sometimes a noisy map will be assigned a color but it will not influence the mix Ifa map has not been assigned a color it either has too much noise or enough different maps have already been found to provide a good mix In the case where 222 EDS SEM The Business of Science there are many different materials in the field of view it is worth checking those maps that hav
384. red image You can also minimize some of your maps to give you a clearer view Map Tools You can use these tools to change the appearance of the maps Description Sets the number of maps per row in the Standard and Interactive displays Offers a choice of map dis play Links images for manip ulation of all layers using the Pan or Zoom controls Unlinks images You can manipulate individual lay ers using Pan or Zoom con trols Changes the brightness and contrast of the cur rently selected image or map 463 Adds or removes a map in the layered image The Lay ered Image icon is in the top left hand corner of the map A symbol rep resenting the map appears on the layered image Minimizes a map The Mini mize icon is in the top right hand corner of each map This is useful if you have too many maps in view The map moves to the Minimized Map tab below the displayed maps Deletes a map from the analysis completely This icon in the top right hand corner of each map Restores a minimized map to its normal size The mini mized maps are on the Minimized Map tab below the displayed maps Map TruMap Sets the mapping mode for X ray Element Maps Automatically adds maps to the layered image This is the Autolayer feature Changes the brightness and contrast and gamma for all the maps Constructing new EBSD images To construct a new EBSD image 1 Expand the Construct EBSD Ima
385. rently available in the Data Tree It can be from any Project any Specimen and any Site of Interest currently available in the Data tree To choose the comparison spectrum click on the down arrow Spectrum 2 in the above example Spectra available in the current Project Soecimen and Site of Interest are displayed as below Project 1 Speamenil Srel 112 EDS SEM CK HE INSTRUMENTS The Business of Science Click on the spectrum in the display to select it for comparison The selected spectrum will be overlaid as a line spectrum over the current spectrum The MiniQuant results are displayed in a table as shown in the example below Spectrum 1 Spectrum 2 The results are displayed as wt weight The statistical error is displayed as o weight sigma for the calculated wt It is the overall confidence figure for the analysis You can use sigma to assess the results especially when an element is present at low concentration For example if an element concentration is 0 2 wt and the ais 0 12 wt the element might be detected at a statistically significant level if the acquisition time for the spectrum is extended If the a is 0 4 wt it is pointless to extend the acquisition time and it is safe to assume that the element if present is at a level above the limit of detection for this technique Press bas to display the results in a chart Spectrum 1 Spectrum 2 Br Weight 113
386. results Quant Results Details You can see the settings used for calculating the composition in the Quant Results Details list box Parameter Description Label Spectrum Label E g Soectrum 1 Element List Type Current Spectrum Fixed List or Combined List 333 Parameter Processing Options Ratio Standard Element Ratio Standard Line Specimen Thickness Specimen Density Automatic Line Selection Thresholding Deconvolution Elements Pulse Pile Up Correction Detector File Description All Elements or Oxygen by Stoichiometry Silicon K Series x nm X g cm Enabled or Disabled Enabled or Disabled None Selected Enabled Disabled Indicates file that has been used to char acterize detector Efficiency Calculated File based Quant Results View The information displayed in the Quant Results View depends on which template has been selected You can view Spectrum Details Spectrum Processing and Diagnostics table in addi tion to quant results See Also Quant Settings below Element Lists on page 191 Compare Spectra amp MiniQuant Results on page 318 Quant Settings The Quant Settings are described below Processing Options To make the correct selection a little knowledge of the specimen is required For example can all elements in the specimen be detected and analyzed or are you analyzing a mineral where it is more usual to calculate the oxygen present e All Elements 334 INSTRUMENTS
387. results in a chart Spectrum 1 Spectum2 Br Weight The sigma values are displayed as black or white vertical bands across the bars in the chart results as shown in the example above In this case the full scale of the bar chart is 50 If you wish to change the MiniQuant Settings press Ed 197 All Elements Spectrum 1 Oxygen by Stoichiometry Spectrum 2 Fe Element by Difference EB Normalize Results Apply Br Weight Make your selection by clicking on the radio button and then press the Apply button The results will be updated immediately Note The Quant Settings in the MiniQuant and Calculate Composition are the same Updat ing one updates the other and vice versa 198 EDS SEM The Business of Science Point amp ID Custom Point amp ID is an image centric application that requires the acquisition of an electron image prior to X ray spectra acquisition There are two modes of operation Guided and Custom In the Custom mode the Point amp ID navigator has three steps Describe Specimen and Compare Spectra are explained in the earlier section The step which is unique to Point amp ID Custom is explained here 199 EDS SEM The Business of Science Acquire and Confirm Acquire and Confirm In Acquire and Confirm step four operations are combined into one window Acquire and Confirm is the main step of the Point amp
388. rface Double click on a peak in the spectrum viewer The candidate elements are displayed in a stacked spectra view on the right hand side of the window you can double click on any of these elements to add or remove it from the confirm elements list You can control what overlays you see in the Spectrum viewer via the Confirm Ele ments Settings These overlays can be very useful in helping you to interrogate com plex spectra Press Include Exclude once you are satisfied with the identification of each element to build your list of confirmed elements Setting up the Search Criteria 47 The section under Composition Used For Search displays the Quant results for the currently displayed Spectrum in Wt and At calculated according to the currently selected Quant Set tings Note that the calculation of the composition takes into consideration the overall tilt of the specimen as entered in the Describe Specimen Step This chemical information forms the basis of the search in the databases However there are some extra settings provided which allow you to optimize the success of your search It is worth noting the following points The EDS system may not be set up for obtaining optimized quantified data under EBSD Conditions as the Specimen is highly tilted You should therefore allow large error margins on the chemical data a Light elements may not be detected Therefore if you suspect carbides bori
389. ring your experiments Right click with the mouse on the Project or Specimen entries in the Data Tree and then select Edit Notes to write modify the relevant notes You can add new Specimens to the current Project by pressing the New Specimen button New Specimen Specimen 1 Note that you may write notes about each Specimen and save them EBSD The Phases for Acquisition are listed in this view together with the number of reflectors color and the option to include exclude them during analysis EDS You can add coating information for each specimen This information is used later during the calculation of the quantitative results Specimen Coating Information E The specimen has been coated with Carbon Y Thickness nm Density g cm3 413 To specify a coating element check the coating option and select an element from the Peri odic table Type the thickness and coating density so that the software applies a full coating correction when calculating the quantitative results The default element is Carbon with the default values for thickness of 10 nm and a density of 2 25 g cm3 The default density of the element is at room temperature and pressure where appropriate You can change the thickness and density if required The peaks for the coating element are automatically deconvolved from the spectrum before quantification but are excluded from the calculation of composition Please see the topics on Speci
390. rnatively press Auto to automatically adjust the exposure time to achieve a signal strength between 85 and 95 see below The Nordlys detector whether NordlysNano or NordlysMax allows you to adjust the quality of the diffraction pattern to suit the particular type of analysis Binning By clustering groups of pixels binning it is possible to collect lower resolution EBSP s at higher speeds Depending on the detector used various binning options are available The table below illustrates the general trend for binning levels and when to use them Binning Suggested Use High resolution EBSPs for posters and publications Regular EBSD anal yses where accuracy Is more important than extreme speed e g phase iden tification 436 Oy 45O ND EBSD INSTRUMENTS The Business of Science Binning Suggested Use Regular EBSD anal yses where speed Is an important issue e g routine grain size amp texture anal yses High speed anal yses where a slight loss In accuracy is not important e g large area texture analyses Camera Gain Adjust the gain level to suit your experiment High gain will increase the sensitivity of the cam era but may introduce more noise as it is the total signal signal noise that is amplified The noise level indicator see below is provided in the application to allow you to look at the effect of adjusting the gain on the quality of unprocessed EBSP and hence w
391. rol Enter a new value into the entry box adjacent to the parameter and press the Set button The column parameters are Magnification Working Distance mm and High Voltage kV which are described below 493 Magnification Magnification is used when calculating the length of the scale marker bar which can be super imposed on an image or the length of a linescan You can change this in the Microscope Con trol window Working Distance mm Working distance is the distance between the point of focus of the electron beam and the final lens i e when this is changed the current through the lens is changed You should ensure that the working distance set on the microscope in millimeters is the desired value for performing X ray microanalysis The recommended value for your instrument is displayed in the Mini View Note that if you change the working distance on the microscope your image may then be out of focus in which case you will need to adjust the Z of the stage to bring it into focus High Voltage kV or Accelerating voltage It is particularly important to have the accelerating voltage set to the correct value since it is used by the quantitative calculation when calculating intensity corrections You can change this in the Microscope Control Stage You can access the stage parameters from the Stage tab in the Microscope Control window Microscope Control Column DefaultMPO Current Values New Values Stage Stag
392. rom a polyphase rock sample Density atomic number Z contrast Polyphase rock sample Orientation contrast How to obtain good FSD images The forescatter detector FSD system is a complementary imaging system to the EBSD tech nique The FSD system is a backscatter detector that uses multiple silicon diodes around the EBSD detector phosphor screen to produce microstructural images The same phenomenon that generates a diffraction pattern generates imaging crystallographic orientation contrast The FSD system provides orientation and phase density Z contrast using up to six silicon diode detectors With a highly tilted sample a typical backscatter detector mounted on the SEM pole piece yields low orientation contrast The FSD system has lower diodes and is well positioned for orientation contrast imaging For some materials sample topography will be observed where the upper and side diodes are positioned for optimal density Z contrast imaging You can enable invert or disable each diode detector signal to achieve the best gray level image 426 EBSD Oy 45O ND INSTRUMENTS The Business of Science A weak signal channel is a common problem with forescatter systems and can usually be fixed by one of the following changes Increase the probe current or accelerating voltage Adjust the sample to detector geometry Check the polish of the sample If the sample gives good EBSPs it will generally also give
393. ron image in Microsoft Word or Excel report a Print prints the current electron image in Microsoft Word or Excel report a Email sends the image via Email Details opens the dialog showing the image details Note You can view reports with the Microsoft Word Excel viewers supplied with your sys tem However Microsoft Office need to be installed for editing your reports Spectrum There are six menu items for each spectrum on the Data Tree Rename Delete Save As Print Email and Details m Rename this renames the spectrum Delete this deletes each spectrum Save As saves the current spectrum in a user selected picture file format a Print prints the current spectrum as an image Email sends the spectrum via Email Details opens the dialog showing the spectrum details Note Hold Ctrl and click on items one by one on the Data Tree for multi select de select Hold Shift and click on children one by one in a branch on the Data Tree for multi select de select Map There are six menu items for Map on the Data Tree Rename Delete Save As Print Email and Details Rename this renames the current map Delete this deletes the current map 39 Save As saves the current map in a user selected picture file format m Print prints the current map Email sends the current map via Email a Print prints the current spectrum as an image Details opens
394. rop down menu in the Database menu The data base list shows the database files present in the CHANNELS directory and will also include user defined databases if present When you have selected a database all phases in the database will be listed Highlight the desired phase in the phase list to view information about the unit cell of the selected phase the phase details and the list of calculated reflectors to the right hand side of the work area The calculated expected intensities of the Kikuchi bands or reflectors are shown in the Reflec tors tab Note that these intensities are given for families of reflectors You can also scroll to a phase in the database by entering the start of its phase name into the space provided It will then highlight the best matching phase in the list Once you have found the phase that you are looking for press the Add Phase for Acqui sition button This will now load the phase into list of Phases for Acquisition and it will be used for indexing EBSPs You may repeat the process and include more phases if you wish 3 D Phase View The 3 D Phase view may be shown with or without the unit cell within the spherical sim ulation of the Kikuchi bands Use the context menu to select different view modes of the 3 D simulation The Kikuchi Map gives a spherical simulation of the Kikuchi bands for the unit cell orientation visible This can be freely rotated using the mouse You may also adjust the appeara
395. rs selected in the Optimize navigator will be used when you start acquiring spectra from your specimen Energy Range keV The appropriate energy range should be selected in conjunction with the current microscope accelerating voltage If the accelerating voltage is above 10 kV in order to view lines which may be excited above 10 keV the 20 keV range should be chosen Below 10 kV it may be more appropriate to choose the 10 keV range since no lines above 10 keV will be excited In the Auto mode the system checks for the accelerating voltage selected on the microscope and sets a suitable energy range in the software Number of Channels Select the number of channels from the drop down list of 1024 2048 and 4096 with which you display the spectrum The number of eV channel will depend on both the energy range and the number of channels you select In the Auto mode the system checks for the energy range selected and sets the appropriate number of channels Process Time Select the Process Time from the drop down list of 1 to 6 The Process time is the length of time spent reducing noise from the X ray signal coming from the ED detector during proc essing By selecting different Process times it is possible to reduce differing amounts of noise The longer the Process Time the lower the noise If noise is minimized the resolution of the peak displayed in the spectrum is improved in other words the peak is narrower and it becomes easier
396. rted into the microscope chamber and ready for acquisition Fully Retracted The detector is fully retracted from the microscope chamber Indeterminate Position The detector is at some position in between the end stops Fault A fault has developed The possible activities that may be displayed are Stopped Moving in Moving out and Auto retracting 485 Protection Depending on the software licenses that you have two options are available to protect your detector from damage by X rays EDS Detector Control Thermal Low Mag Interlock Enabled Position F Enable Flux Protection Protection Delay 5 5 0 Threshold MeV s 480 Low Mag Protection This option is enabled on the X Max detector provided the system has the relevant license Low Mag Protection 06 installed The Low Mag Interlock status is displayed on the Pro tection tab as shown in the screen shot above Putting the microscope into the low mag nification initiates auto retraction of the detector to protect it from the X rays Note that the microscope needs to have hardware interlock for Low Mag Protection to work When the user switches out of low magnification mode the detector will need to be moved back into the chamber by pressing the In button Flux Protection The Flux Protection is only available if appropriate license Detector Flux Protection 05 is installed A checkbox for enabling disabling this option is available on the Protection tab
397. ruct workspace You can acquire element maps here and view them in three different ways Standard Interactive or Summary view To get details of all the functions follow the Acquire Map Data link below Spectrum Viewer The bottom left quadrant displays the current spectrum It can be a Sum Spectrum or a Reconstructed Spectrum At the top right corner of the Spectrum Viewer there is a link to the Confirm Elements step of the Point amp ID Navigator It is a useful option for identifying and confirming small peaks in the spectrum Select Map to get back into the Acquire and Confirm workspace from the Confirm Element screen Selected Element Details 387 The Map Details is located in the bottom right quadrant of the workspace From the Selected Element Details you can select which elements you wish to map You can define the energy windows for window integral maps and select the X ray lines you wish to use for mapping instead of using the automatically selected energy window and lines When you select a map from the element map display the energy window and X ray lines markers for this element are displayed in the spectrum viewer To read details of defining energy windows and choos ing X ray lines follow the link to Construct Maps topic below See also Acquire Map Data on page 363 Construct Maps on page 3 0 Acquire Map Data Settings on page 211 Context Menu Map Viewer on page 223 388 EDS TEM The Business of Sc
398. s 2 In the Reconstruct Spectra dialog select a binning factor 3 Click START to extract the spectra for the points into the project The data is saved in the Data Tree with this icon See Also How binning affects the quality of your data on page 373 402 EDS TEM OXFORD INSTRUMENTS The Business of Science Construct Linescans S _ Construct Linescans In this step you can define energy windows and configure X ray line series to update the dis play of element linescans in the viewer You can use AutolD for initial display and then add or remove elements as you wish using the periodic table and the controls available in the Linescan Details dialog Linescan Details seyd uawa paalas Indude i E Clear Al In addition you can view the Line Sum Spectrum and navigate to the Confirm Elements step from within the Construct Linescan step to manually confirm elements 403 Te aa Line Sum Spectrum 4 Fe Fe Ti 2 4 6 keV Manual selection of energy windows and X ray lines 1 Press to open the Selected Elements Details dialog Selected Element Details Element Beryllium Label Energy Window Selection Automatic Specify Line Series Specify Energy Window Lower Energy keV 0 071 Upper Energy keV 0 146 Update linescan with changes The default settings are automatic X ray line series and energy window width
399. s Nominal thickness nm 5 Once the layer composition has been entered the concentration type for each ele ment in the layer defaults to Fixed 6 Select the element in the table and then select the desired concentration type from the drop down list of Fixed Difference and Unknown The selection of concentration type depends on whether you know the composition or want to determine it It is important to consider carefully what to define as unknowns because choosing too many unknowns will prevent the software from obtaining a solution Fixed If Fixed concentration is specified for an element this means that the concentration is known However when performing the sensitivity analysis it is important to enter a per centage tolerance which will be applied to the concentration of that element during analysis Note that the tolerance is a relative not an absolute parameter For example if the con centration of an element is 60 the tolerance of 10 allows the concentration to be 60 6 Difference This option can be used if you are able to analyze all elements except one The concentration of the element selected as Difference is not measured but is calculated assuming that the difference between the analyzed total and 100 is due only to the presence of this element 271 Intensity corrections are then calculated assuming the presence of this element It should be noted that the total from this type of analysis is al
400. s layer 1 3 Using the Add Above button adds further layers to the layer structure 2 Defining the composition of each layer Enter the layer composition of the substrate first followed by the individual layers The layer details shown on the right hand side of the work space are of the currently selected layer 1 For each layer the composition is specified by one of the two methods either by selecting an entry from the materials database or by manually entering the com position as a chemical formula or in weight 2 When you select an entry from the materials database all the relevant fields for the layer composition will be automatically populated 3 Select the Manual entry radio button to manually enter the layer details 2 6 LayerProbe OXF INSTRUMENTS The Business af Science 4 Toenter the composition choose one of the two modes of entry Number of Atoms or Weight o Selecting Number of Atoms allows the entry of the chemical formula e g Al203 for aluminium oxide o Selecting Weight allows entry by specifying the elements and weight values e g AlI52 93047 07 Layer Details Use material database Manual entry Units Number of Atoms Composition A10 4000 60 Hement Concentration Atomic nominal Wt nominal Al Unknown 40 004 52 930 0 Unknown 59 996 47070 Total Weight 100 000 Al concentration Unknown Density q cm Unknown thickness Fixed thicknes
401. s Dhiecduceudeseuesawaeadaeddeucis 76 Acguire SPEC ga ia pase ere sees ee iss eet i eee tee eee 96 XVII XVIII OITA IY ESIC INC Sasser A ccc tech ded eh hae Ge ahaa aod hereto m lpan and lysed wen klar 115 Calculate Composto Miss oie oct res Sued cumte e eee E E an aS 117 COTO SO CCU ee a ta ath he te Ace ra ey einen ee 120 Analyzer CUS TON 2 44 02 rote tet ot i ee ett tout Cass eeu Aten aR 122 Acquire and Commis 05 duet otasedenobedsledeiweehadesbunbeidebeasrdsedieudaugowlackaes 123 Pont GUID Guided atch eee beatae een aO tok cecd se SAAE EEIEIEE 124 eerca DEE eae a ee ee ao A ae Tee ee ee oe ene 125 Acguire SPE Gaga ln Sia ie hh bce eta netiee atelier arr a use tess 146 Conu EEmMmEN S Bosc ceicys co eras E E 170 Calculate COMPOSITION 2 cee cece cece e ee cece cece cc eeecceeeceeeeeeeeeeeeees 185 PONE Ce DS CUS COMM gee eittatie tna A E 199 ACQUIRE ald Conine eceran EnA a EER 201 Recommended way of working in Point amp ID Custom Mode 22 2 202 Map G lded oeae eee a a a a N Re a e a ee 204 Acguire Map Data ori ears tite ied adelante ea endea ae a EAEE a 205 Construct Ma PSren heat tae ee Cen a TI A A T 219 Analyze Phases onser ett iat ated Sites aer a a AN 226 Wie CUSTOM aa a a aaa aaa ee heute acted oatet 236 Acguireand Construct os c Coven oot Sheth vad abe aa E E A 237 LIN CSCO GUIGC iiss coated etecniae und ciunnlaenetassunthanden Giana stneushaselseatamanei ations 239 Acquiring liNescanS
402. s Explorer Launches Oxford Instru ments s home page Provides access to System Info Assembly Info and Credits Getting started Oy 45O ND INSTRUMENTS The Business of Science Preferences You can change the appearance of many parts of the software to suit your own needs by recording your preferences on the Preferences dialog The software saves your preferences on the computer that you are currently using When you run the software again it has the appearance that you prefer Your preferences will not be available if you run the software on a different computer or with a different logon on the same computer Setting your preferences 1 Click the Tools menu then click Preferences to open the dialog Preferences Auto Save Report Image Scaling Pixels Per Inch EBSD 3D Phase Viewer Show Acquisition Areas in Reports Show All Show Selected Show None EBSD Image Viewer EBSD Pole Figure Viewer EDS Layered Image Settings EDS Linescan Viewer Package Templates EDS Spectrum Viewer Image Viewer INCA Image Export Reports Status Bar Welcome Screen EDS SEM Point amp ID Template Layer Map Layer Map A4 xlsx EDS TEM Point amp ID Template Electron Image Spectrum Electron Image Spectrum Ad docx EDS SEM Map Template Maps L Maps A4 L docx EDS TEM Map Template Maps L Maps A4 L docx EDS SEM Linescan Template Linescan Tiled Linescan Tiled Ad idocx EDS
403. s and move the spectrum along the horizontal axis To expand the spectrum along the horizontal axis with Pan tool selected hold down the Ctrl key while dragging the spectrum with the left mouse Normalize Spectra You can normalize two spectra over a selected point or a region Normalize Spectra Point i74 4760 FD or INSTRUMENTS The Business of Science You have the current spectrum in the spectrum viewer Select the second spectrum using the Compare drop down The second spectrum is overlaid on the current spectrum Select the Normalize Spectra Point option from the toolbar The cursor turns into an up down arrow a Double click in the spectrum to set a normalization point along the X axis A win dow is drawn on either side of this point Both spectra are scaled along the Y axis to the average value usually cps eV in the window Normalize Spectra Region You have the current spectrum in the spectrum viewer Select the second spectrum using the Compare drop down The second spectrum is overlaid on the current spectrum a Select the Normalize Spectra Region option from the toolbar The cursor turns into a crosshair Click in the spectrum viewer to select the start point of the energy window A default window is displayed about this point Drag the mouse to define your win dow and then release it A window will be drawn between the first point and the end point where you release
404. s in the image appear white 5 Continue making adjustments as in the previous steps until you obtain a good image 6 Adjust the Weight control to include this image in the Mixed image How the FSD gain and offset controls work The FSD diodes generate a range of signals as they detect electrons emitted from the sample during scanning The signals are processed by electronics before reaching the software for further processing Depending on conditions of the microscope and the sample the range of diode signals might be small When the image is subsequently viewed its correspondingly small range of grays might make some features difficult to see Although you can adjust the contrast and bright ness using the software the results might be disappointing For a clear view of the features in the final image you need a wide range of signals from the detector to give with a wide range of grays from nearly black to nearly white 431 For example the diode output gives only a small range of signals somewhere between zero and a maximum E The equivalent range of grays is small The electronics can apply an offset forcing the same small range of signals to start at zero B Although the equivalent range of grays is still small it now originates with black The electronics can also apply a gain to increase the range of signals This increases the equivalent range of grays such that the maximum signal is equiv
405. s section appears only if a forward scatter detector is correctly configured To control set tings for the signals from the forward scatter detection diodes click the Settings button to open another dialog If you select the Auto checkbox before you start a new FSD acquisition the software auto matically adjusts the signal from each diode for optimal brightness and contrast The opti mized electron image then appears after a delay of a few seconds When you first start the software the Auto check box is already selected for you See Also AutoLock on page 133 Scan Image on page 418 Scan Image Toolbar The Toolbar is located near the top left side of the Scan Image window Tools are provided to manipulate and annotate the image 130 EDS SEM OXF INSTRUMENTS The Business of Science Pan and Zoom You can move the image using the Pan tool Use the wheel mouse to zoom in and out Annotation There are five different tools to add annotations on the current image as shown in the screen shot below To edit an annotation double click on it to select it the editing handles will be displayed Use the handles to edit the annotation To delete an annotation select it by double clicking on it and then press the Delete key on the keyboard To delete all annotations on an image choose Select All from the Annotations context menu on the image viewer and then press the Delete key on the keyboard Inform
406. s tab shows the combination of images that you select from the many phase maps and the electron image The spectrum bottom left shows a spectrum extracted from the pixels in the cur rently selected phase You can also closely examine the spectrum at any point or area of interest using tools on the left toolbar a Phase Details bottom right shows the area of each phase in pixels and as a per centage of the total area of the map You can copy these results into a spreadsheet Toolbars around the window enable you to change the processing of the data and display and analyze the data See Also About phase maps on page 377 Analyze Phases toolbars on page 383 Sol a Finding phases In the Analyze Phases step the software automatically converts X ray maps into phase maps The phase maps help you to see the constituent elements of the phase and how the phases are distributed over the specimen You can run this step while map data is acquired or after wards If map data is being acquired the phase analysis repeats periodically until acquisition finishes or you click the Cancel Processing button The phase analysis produces the best results if run after all the map data has been acquired and elements have been identified 1 See Also In the acquisition toolbar click the green Find Phases button to start processing When processing is finished phase map data appears on the Data Tree for exam ple 1 Ti
407. s the length of time spent reducing noise from the X ray signal coming from the ED detector during processing By selecting different Process times it is possible to reduce dif fering amounts of noise The longer the Process time the lower the noise If noise is mini mized the resolution of the peak displayed in the spectrum is improved in other words the 314 EDS TEM OXF INSTRUMENTS The Business of Science peak is narrower and it becomes easier to separate or resolve from another peak that may be close by in energy If Default is selected the Process Time is automatically set to a suitable value There is a trade off between the Process time that is used and the speed at which data can be acquired into the X ray spectrum Process time 1 is the shortest and as such gives the highest X ray acquisition rates but at some cost to resolution Process time 6 is the longest and gives the highest resolution but at some cost to maximum acquisition rate The longer the Process time the slower data can be acquired i e the higher the system Deadtime will be for a given input count rate The input rate is not affected by the pulse processor Which Process Time should I use When you start your application first time the Process Time is set to Default This is a suitable choice for many routine applications where you are looking for good resolution of peaks and fast acquisition For the first look at a specimen you should
408. saving to profiles Wrong values of pre tilted specimen holder were used during EBSD mapping under certain circumstances system uses tilt value from previous map a Occasional connection errors to EBSD hardware Vill What s New in Version 2 0 The Business of Science What s New in Version 2 0 Following are new features and enhancements included in this version of the software AZtecTEM The main focus of AZtec 2 0 has been the introduction of AZtecTEM software Improvements to reporting The way the report templates are created has been improved a Ability to edit create templates Increased number of report templates to choose from 350 Pee Cee bermas Tii iene Lee LE a Site report Users will have the ability to print a combined report of all data objects in a project with just one click EDS and EBSD data Eril Report Templates Company logo The company logo can be changed for all templates simply by copy ing the logo image file into the following directory C Program Files Oxford Instru ments NanoAnalysis AZtec Reports _ix Annotations on spectra annotations on spectra are now Saved in the project and will be visible on report templates J eere sirin n mme en 1 L Ea eiee ie mi a SIRO OL SIEHE AARM TE ma F E J U ow Wa tA EET IPCA a Thera Toto Heading y a od Fert a HUE a ohh p a pwns grr peheied i Brust 4 es ee hee 4 ibt tee ce Ta
409. screen shot below necimen Geometry Pre defined Elements Press this to load a profile for your Load from Profile analysis Predefine your elements from the Periodic table Click on an element first to select it and then press the Include button save to Profile h Na Mg Si Po ay k a S rh Y Cr Mn l gt rear Mo e h Pd n g Save the Predefined Elements to the User Check this box to Profile enable AutoID during the spectrum acquisition Np Pu Am l Include h E Perform Auto ID During Acquisition Note that the Pre defined Elements are saved with the current Specimen Changing the Predefined Elements will only update the Pre defined Elements in the current Specimen It will not update any existing Specimens in the Project 162 EDS SEM OXF INSTRUMENTS The Business af Science Data View Current Site Data Tree s Project 1 P a Specimen 1 dg Specimen 2 4 gt Site _ Electron Image 2 Spectrum 9 Spectrum 10 Spectrum 11 a P p 3 4 Site3 Electron Image 3 Spectrum 1 Spectrum 13 Spectrum 14 The current specimen is the one that you are presently analyzing processing the data from For example in the screen shot above Specimen 3 is the current specimen Spec imens 1 and 2 are the other specimens in the Project Identified Elements The Identified Elements will include a Any Pre defined Elements Elements identified by Auto ID a Any addition
410. se and you are ready to snap a pattern As described below if Auto is checked a pattern will automatically be snapped but if it is not you should then press the Snap button If you wish to release the beam back to SEM control press Off In addition to acquiring a live EBSP by positioning the beam you may wish to optimize the solver settings based on EBSPs from previously acquired EBSD Maps It is often very useful to check the solver settings before setting up an area for reanalysis In the same manner as described above select the Extract EBSP from EBSD Map tool on the toolbar This tool will allow you to place the cursor on the map and extract the EBSP from the specified position When the cursor is placed the EBSP is automatically extracted If the Auto function is enabled then the band detection and indexing will automatically take place Band detection and Indexing of the Processed EBSP Auto By enabling Auto the system will automatically snap a live EBSP detect the bands and try to index with the selected settings It will also automatically update whenever a change is made to beam position the EBSP the detected bands or the analysis settings and phases If you do not select Auto you must press Snap Detect and Index in order to go through the steps of snapping a pattern detecting the bands and indexing the pattern Load EBSP This function allows you to load an EBSP from file together with its calibration and acquisiti
411. se to store EBSD patterns without solving them in order to analyze them later Once this saving option is selected under Settings you may proceed to acquire Map data without having to first select the candidate phases How to Acquire Maps The default way of selecting an area to map is by using the Map Area Calculator tool which is selected by default as you enter this step This tool allows you to link the acquisition time step size and area of a rectangular map region Alternatively to acquire map data from a region select the required map acquisition tool from the standard region Rectangle Ellipse and Freehand tools available from the toolbar If you wish to do a full area map select any of the region tools and press start If you wish to select a reduced area map select one of the standard region tools click on the image and drag with the left mouse to outline a region on the image Maps will then be automatically acquired from the scanned region on releasing the mouse Using The Map Area Calculator If you cannot see the calculator above the image click the Map Area Calculator tool icon on the toolbar on the left of the image The shaded box on the electron image shows the location and size of the area to be mapped The Map Area Calculator tool works with the settings that appear above the image You can position and resize the area using your mouse and the following controls Duration Locks the acquisition time While you defi
412. sed for the calculation of quantitative results In the default Quant Standardizations file some low energy lines have been deliberately omitted because there are many potential sources of error for quantification For example close overlaps chemical shifts anomalous excitation and absorption effects on individual lines inaccurate absorption coefficients and presence of carbon and oxide layers that give large peaks at low kV If you understand the issues you can still use your own standards to perform analysis for these lines However they have been omitted from the default file At low kV fewer x ray lines are excited and if the recommended line is not available quan tification is not possible In this case the spectrum overlays cannot be calculated and will not appear in the Confirm Elements step If you want to work at low kV the factory stand ardizations file Quant Standardizations Extended Set has additional low energy Land M lines that will allow you to obtain a concentration result and enable the spectrum overlays You may find it convenient to use the same file at both high and low kV but it is important to realise that concentration estimates obtained using these extra low energy lines may some times be inaccurate Apply and Save If you make a change to the Quant Settings and press the settings are saved and the currently selected spectra are quantified The quant results are updated imme diately Save If you
413. sed ie Bi hea as A 377 VIG FONG DNS CS coast ee ee ee ee tr eerie eee an 379 Phase maps in the Data Tree 2 0 eee cece cece e cece eee cceecececeeeeeeues 380 Analyze Phases settings oeoa e Poti ian eed 381 Analyze Phases t olbarS sran Ae R ORAE ERRE 383 Mope U TO aaa aN e ES Cm ee Ree ara ae 386 Acquire and Construct 0 0 c cece ccc e ec cece cece ce eecceeecceecceueeceeeceeees 387 Linescan Guided ieee ch inbound kacandateabantednctinds seckuintiiahtet arante wien sanene 389 ACOMIFING MNMES CONS cot ssisekhoet cocoa Glatt Ae eee ea a eau hae aO ese 391 Displaying and manipulating linescans 0 222 c ieee cece eee eee cece eee ee 393 Measuring the distance between two points 0 00 2 c eee cece eee eee cece eee 395 Viewing element counts and percentages 2 22 eee eee eee eee ee cece eee ee 396 Comparing element quantities 0 0 0 0000 c lee eee eee eee cece ee eee eens 397 Smoothing TNEIINGSCANSs 2 geen giiliwe es vento axe diel NU wsteveundzeieuauel en asenda cbse 398 LIMES GAN Dales 4 aectn need took Sot ation EE E eee EEES 399 Exporting the linescan data 00 0 022 c cece cece cece eee cece cece eee e eens 400 Extracting a single spectrum from the linescan 2 0 222 eee cece ee eee eee eee ee 401 Extracting multiple spectra from the linescan 2 222 e cece eee cece eee eee 402 Construct TINGS CAINS 5 25355 aes user tt oienecis ie EE EEN E 403 LUNES CAN CUStOM
414. selec tion 404 OX FO RID EDS TEM INSTRUMENTS The Business of Science 2 To manually define the width of the energy window check the Specify Energy Win dow option Enter the values for Lower Energy keV and Upper Energy keV and m Update linescan with changes press 3 To manually select the X ray line for an element linescan check the Specify Line Series option Select the line from the Line Series drop down list and press Update linescan with changes d Linescans Display There are three different display options available from the controls near the top right corner of the Construct Linescans screen Display image full screen Display linescans and image Display linescans full screen See Also How binning affects the quality of your data on page 373 405 Linescan Custom In the Custom Mode the Linescan navigator has two steps The Describe Specimen step is explained in the earlier section The new step is described below Acquire and Construct Linescans 22 222 222 eee ee eeeee 407 406 EDS TEM Oy 45O ND INSTRUMENTS The Business of Science Acquire and Construct Linescans Acquire amd Construct The three components Scan Image Acquire Line Data and Construct Linescans are laid out as separate steps in the Guided mode of the Linescan application These three components are combined in the Custom mode to
415. set the number of reflectors for each phase you can set a maximum This means that the closest value to this maximum while still being lower will be automatically found for the number of reflectors for each phase You can then manually change it after wards Note that changing the maximum value will automatically trigger another update of the reflector values for each phase Exclude phases from list In situations where there are a number of phases found it may be useful to exclude some of the phases from the list Uncheck the phases you wish to exclude when indexing the EBSP In order to make a potentially long list of phases more readable you may wish to display only the included phases This can be controlled from the Show excluded check box Choice of EBSP The EBSP displayed in the image viewer corresponds to the current EBSP the one displayed under the highlighted Point Data node Highlight a different Point Data node in order to dis play another EBSP Alternatively select the required EBSP from the drop down list box posi tioned above the image viewer This EBSP might have been acquired at a different time or from a reconstructed point Use the drop down list box to pick an EBSP that is acquired at a different time point than the highlighted spectrum 480 EBSD The Business of Science Indexing the EBSP There is no limit to the number of phases that can be used for indexing However the greater the number
416. several ways a Line also known as Window Integral obtains the counts in the element energy win dows including the background Line gives a fast and simple representation of the X ray energies TruLine also known as Filtered Least Squares FLS applies further processing Sometimes the standard X ray mapping Line gives misleading results because some elements have overlapping energy windows For example a Titanium linescan 239 240 might include Barium information The TruLine option eliminates the problem by comparing the X ray line series with the expected peak shape for each element The linescans are corrected for peak overlaps and any false variations due to X ray back ground QuantLine further processes the data showing the atomic or weight percentages of elements at every point on the line EDS SEM OxKFC INSTRUMENTS The Business af Science Acquiring linescans The elements for which linescans are being acquired are chosen in the Describe Specimen step by selecting the Auto ID option Pre defined Elements or both To see the acquisition settings click the Settings cog in the toolbar in the title bar 1 Select man the Acquire Line tool from the toolbar on the left 2 Click on the image to set the start point and then drag the mouse to define the line Release the mouse to set the end point A line with start and end points is defined on the image START o a 3 Press to start acqu
417. sible states are shown in the table below State Description Standby Cooling is powered down Allows power save and detector lon gevity Steady orange LED Warm Detector is not ready for data acquisition Steady orange LED Cool Detector is ready for data acquisition Steady blue LED Warming Detector is warming after selecting the Standby mode Cooling Detector is not ready for data acquisition Flashing blue LED Fault A fault has developed Red LED 484 Hardware Control OXF INSTRUMENTS The Business af Science There are two buttons in the Thermal Control tab Operate and Standby Pressing the Oper ate button initiates the cooling process When the detector is not in use pressing the Standby button puts it in the Standby state Note If the detector is not cold or it is in the process of cooling the spectrum acquisition will be disabled Position The Position tab displays the current slide state of the detector EDS Detector Control Thermal State Fully Inserted Position Activity Not Moving Protection Out There are three buttons on the Position tab In Out and Stop Pressing the In button will start moving the detector into the chamber The Out button will start retracting the detector from the chamber and Stop will stop the detector at the current position The possible detec tor states are shown in the table below State Description Fully Inserted The detector is fully inse
418. situations when more than one phase with the same crystal structure can co exist in a given sample In many cases these can be discriminated from each other using chemical information acquired from EDS data but not directly from their EBSD patterns In such cases it is possible to look at the difference in lattice parameter in order to identify such phases of similar crystal structure The software enables phases of the same crystal structure to be discriminated from each other using their respective EBSD patterns using band widths provided their lattice param eters differ by more than 10 A good example of this is Platinum Nickel which have the same crystal structure but have a difference in lattice parameter of 14 The Phase Group Configuration window allows you to group materials together which have similar crystal structures To create groups of phases 1 At the Describe Specimen step select the Phases tab 2 Under Phases for Acquisition click Configure Grouping to open the Phase Group Configuration dialog 3 In the dialog under Ungrouped Phases select two or more phases for the group 4 Click Create Group The new group appears under Phase Groups 5 Create any other groups if required To improve the view of large phase groups you can drag the bottom right corner of the dialog outwards 6 To remove a group click the X in its top right corner To delete all groups click Remove All Groups 7 C
419. sity information in a BSE image on the secondary electron SE image Remove all other maps from the layered image Ensure that the map display is set to Interactive Below the BSE image use the drop down list to change the color of the BSE image Below the BSE image select the Mix layer mode a e WwW N FP Adjust the brightness and contrast on the BSE image to emphasize the layered image as required 217 Itim 2210 EDS SEM The Business of Science Construct Maps Construct Maps In this step you can select which elements to map and which ones to exclude You can change the default X ray line used for Window Integral Maps for any given element It is also possible to define energy windows whose widths you can specify yourself rather than using the auto width calculation Tools are provided to interrogate the map data to confirm the elemental composition of user specified areas of interest You can navigate to the Confirm Elements step from within the Construct Maps step To reduce the effects of noise in the maps you can apply a binning factor Map Details Map Details dialog allows you to choose elements you wish to include or exclude for map ping You may have pre defined the known elements in your specimen in the Describe Spec imen step You can map these elements by pressing the Pre defined button in the Map Details dialog There may be unexpected peaks in the spectrum You can use AutoID for
420. ss time that is used and the speed at which data can be acquired into the X ray spectrum Process time 1 is the shortest and as such gives the highest X ray acquisition rates but at some cost to resolution Process time 6 is the longest and gives the highest resolution but at some cost to maximum acquisition rate The longer the Process time the slower data can be acquired i e the higher the system Deadtime will be for a given input count rate The input rate is not affected by the pulse processor Which Process Time should I use When you start your application first time the Process Time is set to Default This is a suitable choice for many routine applications where you are looking for good resolution of peaks and fast acquisition For the first look at a specimen you should use a long process time 5 or 6 to start with in order that you do not miss any detail in your spectrum For example when identifying peaks particularly those closely spaced and overlapping it is important to get good peak sep aration Good resolution is also important for looking at a series of lines that are very closely spaced like an Lseries and process times 4 to 6 should be chosen Common overlaps include the Mo Land the SK lines If there are no closely spaced peaks then you can afford to use a shorter Process Time such as 1 3 which will enable you to increase the acquisition rate by increasing the beam current A compromise between acquisition speed an
421. st of elements I am not interested in any other ele ments may want to see their labels on spectra their X ray maps or both I want to see these even if the element is not present I know what s in my sample I want to look for a specific set of elements I want to see these even if the element is not present but I would like to know if there is anything else in my sample too You can define these elements in the Pre defined Elements tab in the Describe Specimen step If you want to save the Pre defined Elements to a profile you must first press Save to Profile button then save the profile via the drop down menu When you want to analyze your Specimen you can load this profile or another profile by pressing the Load Profile but ton in the Describe Specimen step as shown in the screen shot below 176 EDS SEM OXFORD INSTRUMENTS The Business of Science Specamen Geometry Pre defined Elements Press this to load a profile for your Load from Profile analysis Predefine your elements from the Periodic table Click on an element first to select it and then press the Include button Save to Profile Na Mg ies a K Ca Sc oH Y Cr Mn ni E Sr Y E Ab Wo Ta R ch Save the Predefined Elements to the User Check this box to Profile enable AutoID during the spectrum Pm acquisition Np Pu s Include 5 E Perform Auto ID Dunng Acquisition Note that the Pre define
422. surface is well prepared 428 EBSD Oy 45 O ND INSTRUMENTS The Business of Science Sample is too high Sample is correctly placed Sample is too low If the sample is too close to the diode detector the signal is shadowed by the sample If the sample is too far from the diode detector the signal is weak A small change in geometry can often significantly improve the image quality Collecting an FSE image 1 In the acquisition toolbar above the electron image and below the Navigator click Settings Settings 2 On Scan Image Settings select your electron image s scan size dwell time and input signal 3 At Input Signal tick a box to capture the forward scatter electron FSE image 4 Enable Auto to automatically optimize the gray levels of the FSD diode channels 5 Click Start to collect the electron images After your FSE image has been collected the data tree creates the FSD Data folder where it stores all data related to your FSD system The FSD Channels folder stores each collected image channel The number of channels on the data tree depends on the physical number and position of FSD diode detectors for your FSD system 429 FSD Data 3 a ee Upper Left 3 Upper Right 3 Lower Left 3 Lower Right 3 side Left 3 Side Right 3 FSD Mixed Image 3 See Also Scan Image Settings on page 421 Data Tree on page 85 FSD data Scan Image on page 418 Optimizing
423. survey of ahomog enous specimen Rectangular Click on this icon to select the Rectangular Tool Click and drag the mouse on the image to outline a rectangular area When you release the mouse button an area will be outlined and a spec trum will be acquired from it This is a useful tool for examining regular shaped features and areas on an image 150 EDS SEM Ellipse Click on this icon if you wish to define an ellipsoid area on the image Click and drag the mouse on the image to outline an area When you release the mouse button an area will be out lined and a spectrum will be acquired from it This tool allows you the flexibility of outlining an oval or ellipsoid feature on an image Freehand Click on this icon if you wish to acquire a spectrum from an irreg ular shaped feature on the image Click and drag the mouse around the feature on the image Once you have defined the fea ture release the mouse button A spectrum will be acquired from it Acquire Spectra Toolbar The Acquire Spectra screen has a toolbar on the left side of the workspace shown in the screen shot below s151 Pan Tools to pan normalize and _ add annotations Drop downs with alternative options Tools to specify points and regions on an electron image for spectrum acquisition Tools to specify points and regions on a Layered Image or SmartMap for spectrum reconstruction fl ES N 4 l
424. t included in the phase name So ay BC EN CY SL WL PLE PL ea 0 3 10 15 keV The names of the cations and anions are arranged in an order that closely resembles the name of a chemical compound The name of the phase is a possible indication of a chemical compound The order of the phases The order of the phases depends on the distribution and quantity of each group of elements The first phases indicate large areas of closely grouped elements Later phases show smaller areas that are more thinly distributed for example a 2SiO shows one large area or a few large areas that contain Si and O a 24 SiO shows smaller and probably more scattered areas that contain Si and O The number of phases You can display more or fewer phases by changing the analysis settings or by merging phases manually See Also 228 EDS SEM The Business of Science Analyze Phases settings on page 381 Merging phases on page 379 Merging phases To simplify the results of the phase analysis you can merge some phases The result is a new phase with a combined spectrum and fewer phases overall For example these phases have similar spectra and might be considered to be the same phase You can merge similar phases in several ways Seta higher Grouping Level to automatically combine any number of similar phases a Manually merge any two phases To manually merge two phases 1 Inthe phase maps select a phase 2 R
425. t spectrum and Spectrum 2 is the comparison spectrum You can select the comparison spectrum from a Project currently available in the Data Tree It can be from any Project any Specimen and any Site of Interest currently available in the Data tree To choose the comparison spectrum click on the down arrow Spectrum 2 in the above example Spectra available in the current Project Specimen and Site of Interest are displayed as below 166 EDS SEM ON INSTRUMENTS The Business of Science Proect1 Speamenil Click on the spectrum in the display to select it for comparison The selected spectrum will be overlaid as a line spectrum over the current spectrum The MiniQuant results are displayed in a table as shown in the example below Spectrum 1 Spectrum 2 3 Wt c W o The results are displayed as wt weight 167 The statistical error is displayed as o weight sigma for the calculated wt It is the overall confidence figure for the analysis You can use sigma to assess the results especially when an element is present at low concentration For example if an element concentration is 0 2 wt and the ais 0 12 wt the element might be detected at a statistically significant level if the acquisition time for the spectrum is extended If the a is 0 4 wt it is pointless to extend the acquisition time and it is safe to assume that the element if present is at a level above the limit of detection for
426. t the analysis period Therefore the correction works best when analysis is per formed on single pixels points or areas of same composition Bad results may be obtained if the beam is rastered over an area where composition is changing or if a spectrum is recon structed from a SmartMap over a region where the composition is changing Acquire Spectra Toolbar The Acquire Spectra screen has a toolbar on the left side of the workspace shown in the screen shot below 99 Tools to pan normalize add annotations and show data values Drop downs with alternative options Pan The Pan tool allows to expand the spectrum along the vertical axis and move the spectrum along the horizontal axis To expand the spectrum along the horizontal axis with Pan tool selected hold down the Ctrl key while dragging the spectrum with the left mouse Normalize Spectra You can normalize two spectra over a selected point or a region Normalize Spectra Point You have the current spectrum in the spectrum viewer m Select the second spectrum using the Compare drop down The second spectrum is overlaid on the current spectrum Select the Normalize Spectra Point option from the toolbar The cursor turns into an up down arrow Double click in the spectrum to set a normalization point along the X axis A win dow is drawn on either side of this point Both the spectra are scaled along the Y axis to the average value usually cps e
427. ta is acquired and an EBSD data folder appears in the Data Tree However the folder does not contain images such as Band Contrast and Layered images nor details such as the solver settings and hit rate because no solved patterns have been stored Note that you cannot export this project data to CHANNELS for analysis because the project contains no solved data See Also Acquire Map Data Settings Display Modes and Map View Settings The settings are described below Display Modes You can view maps in several different modes using the drop down list on the Display tool bar a Standard a Interactive a Summary In the Summary view you can see details of the energy window and X ray line used for each EDS map if you have selected to acquire EDS maps with your EBSD data Other details include the Layer Name Map Color where appropriate and whether the map has been selected for the Layered Image Map View Settings You can manipulate and view the data by using the Settings dialog Di Settings Image Layer Settings sort Order Maximum intensity Layer Visibility Selection Manual Auto maximum intensity smoothing Level E ACE while acquiring 460 Sort Order EDS Layer Visibility Selection EDS Smoothing Level EBSD Description Sorts the map in several ways Alphabetically By atomic number a By maximum intensity in map sorts on the value of the bright est pixel in c
428. te and Standardize The Calibrate step is described in an earlier section The Standardize step is described here Standardize 2222222020222222 263 262 EDS SEM Oy 45O ND INSTRUMENTS The Business of Science Standardize The Standardize application allows you to setup your own standards for quantitative anal ysis It is accessed from the Optimize navigator File View Techniques Tools Help ai Optimize ee EDS SEM Standardize F Use the links below for further details about Why Standardize below Getting Started with Standardization on page 265 Managing Standardizations on page 267 Why Standardize Quantitative analysis can be performed without the need to measure standard materials since your system is supplied with a complete set of default standardizations However in spe cific cases using your own standards will lead to an improvement in your quantitative results The purpose of Standardize is therefore to enable you to set up your own standards for quan titative analysis When you use your system for the first time and click on the Standardize step your own standards database will be created At this stage your database will contain only the Factory standardizations Once you have standardized entries your standards data base will be modified accordingly Quantitative analysis of elements in any Specimen requires an accurate measure of the inten sity of peaks before th
429. te that standards must be bulk materials Typically you may need to standardize if Accelerating voltages are less than 10kV a You are analyzing light elements You are using X rays lines less than 2 keV The need to standardize depends very much on the level of accuracy you require from your analysis on any one material As a rule of thumb Ifyou require accuracy such that the relative errors are less than 2 you should standardize 290 LayerProbe Oy 45O ND INSTRUMENTS The Business af Science Ifyou are quantifying elements whose X ray lines are in the low energy region of the spectrum which may be the case if you are using an accelerating voltage of less than 15kV or the element you are quantifying has an atomic number less than 11 standardization will improve your quantitative results Ifthe matrix corrections are high such as would be in the case of quantifying Al in a Pd matrix e g light element in heavy matrix or vice versa you should standardize 291 Calculate Layers ccc Calculate Layers This Step allows you to view your quantitative results in more detail using a number of avail able templates It also provides the opportunity to produce tables containing results from multiple spectra Such tables may be exported to third party software for further processing using the Copy and Paste function For multiple spectra statistical parameters such as average composition an
430. that extends from green to yellow to red as the limits of AutoLock are reached the bar will be full and in the red if AutoLock limits are exceeded The proximity value gives the worst case drift range for the acquisition area and the tracking image In extended field mode the tracking image area always determines the proximity as it contains the acquisition area For in field mode either the tracking image area or the acqui sition area determines the proximity depending on which one is closer to the edge of the field See the illustrations under What is In Field Mode and What is Extended Field Mode above What does the AutoLock Histogram show The AutoLock performance histogram shows the number of drift corrections at various dis tances in tracking image pixels that have been applied during a single acquisition the his togram allows a rapid assessment of drift For a stable sample most histogram values should be at or near zero Large numbers of adjustments towards the right of the histogram long distances might indicate that you would benefit from using a shorter measurement interval Context Menus Image Viewer A number of useful shortcut menus available as right mouse click in the image viewer are shown in the table below Context Menu Item Rescale Image Fit Image to Display Fill Display with Image Color Bar Header Scale Bar Show Con trast Brightness Buttons Color Key Set Image Colors
431. the FSD mixed image 1 On the Data Tree highlight the FSD Mixed image E The FSD mixed image and FSD image channels become visible in the image viewer The FSD mixed image displays short labels for the selected FSE image channels For example LL indicates Lower Left D FSD Mined Image 2 Select a mixing mode 430 EBSD The Business of Science FSD Z Contrast uses the upper and side FSD detector channel images Select this mode if you are interested in seeing a density atomic Z contrast signal FSD Topo Orientation uses the lower FSD detector channel images Select this mode if you are interested in seeing an orientation contrast signal Custom Include and exclude FSD detector channel images of your choice 3 In the image viewer do any of the following to obtain a good image Include or exclude individual channels to be displayed in the FSD mixed image Manually optimize the gray image levels to achieve the best contrast and brightness in each channel Add color to the lightest and darkest point in the channel image Optimizing the signal from a single FSD diode 1 In the FSD image find the darkest and lightest features of the image 2 Below the image click the cog icon to open a dialog box Weight Offset Gain 3 Adjust the Offset control to make the darkest features in the image appear black 4 Adjust the Gain control to make the lightest feature
432. the Mini View if you wish to view full size spectrum in the Acquire Spectra step The features of the electron image in the Mini View are The default state is full image with Scale Bar micron marker You can remove the Scale Bar from the display by de selecting it from the image context menu The Context menu items are Show Acquisition Areas Show All Show Selected Show None 41 Show Scale Bar Features such as Pan Zoom and User Annotations are not available in the Mini View Spectrum Monitor It provide a means for the user to see what X rays are being detected at any given moment It is useful for a quick survey of the specimen to find an area of interest for analysis Spectrum Monitor uses the current spectrum acquisition settings with the additional setting of the refresh rate for monitoring the spectrum This refresh time is referred to as the Buffer Size The default is 20 but can be changed under the Settings for Soectrum Monitor in the Mini view Increasing the Buffer Size corresponds to a longer refresh rate The settings in the Spectrum Monitor are Buffer Size The default value is 20 Number of Channels 1024 2048 or 4096 Energy Range keV 0 10 0 20 or 0 40 The settings can be selected from the Acquire Spectrum step or Mini View If you make a change in the setting in one place it is automatically updated in the other Ratemeter It is very useful for setting up the microscope beam current while v
433. the dialog showing the map details Layered Image There are six menu items for the Layer Image Rename Delete Save As Print Email and Details m Rename this renames the Layered Image Delete this deletes the Layered Image Save As saves the current Layered Image in Microsoft Word or Excel report a Print prints the current Layered Image in Microsoft Word or Excel report Email sends the Layered Image via Email Details opens the dialog showing the Layered Image details EDS Data There are two menu entries for the EDS Data Rename and Delete Rename this renames the EDS Data Delete this deletes the EDS Data X ray Map There are six menu items for each X ray Map Rename Delete Save As Print Email and Details Rename this renames the X ray Map Delete this deletes the X ray Map Save As saves the current X ray map in Microsoft Word or Excel report a Print prints the current X ray map in Microsoft Word or Excel report Email sends the map via Email Details opens the dialog showing the Layered Image details EBSD Data There are four menu items for EBSD Data Rename Delete Export and Details Rename this renames the EBSD Data Delete this deletes the EBSD Data Export exports the currently selected EBSD data as a CHANNELS project CPR file or a Channel Text File CTF You may also include EBSPs as TIFF files This option is not available if yo
434. the list of topics by pressing the back arrow near the top left corner of the Help Viewer G EDS SEM The Business of Science EDS SEM Setup for EDS __ 2 8 8 icc cece ccc e cece aaoo araara 65 Calibrate aaa0a0000a00a000000 0000000000000000 aonana 66 Calibration Element 22 2222 2222 cece eee cece eee 70 Calibrate for Beam Measurement Settings 71 aCe OO ioe otto segeeee e ee ee e cee eene ee eae noreuaewuces 72 EDS Qualitative Analysis 20 2222 2222 eee eee eee eee 73 Analyzer Guided 22 22 02 200 22 occ c cece cece cee ee cece eee ee eee 75 Describe Specimen 2 222 222 2 22 eee eee ee cece eeccceeeeeees 76 Acquire Spectra 2 22 22 e cece cece cece cece ec ceeceeeeee 96 Confirm Elements 22 22 2 202 e cece cece ee ceeeeceeeeee 115 Calculate Composition 2 22 2 2222 ee eee ee eee eee ee 117 Compare Spectra 0 222 2 c cece eee ee ee eee eee eee 120 Analyzer Custom 2 222 2 20 0222 2 cece cece cece cece eee e cece eee ees 122 Acquire and Confirm 222 222 22 ecee eee eeeeeceeeeeee 123 Point amp ID Guided _ 8 2 8 cece cee cece eeeeee 124 SCAN TMG anne eRe Se AES 125 Acquire Spectra 2 22 22 eee c cece eee eee ec ceeceeeeeees 146 Confirm Elements 22 222 202 e cece cceecceeeeceeeeee 170 Calculate Composition 22 22 2 2222 eee ee eee ee ee eee 185 Point amp
435. the mouse Both spectra are scaled along the Y axis to the average value usually cps eV in the window Annotations Three tools available to add annotations on the current spectrum are Text Rectangle and Ellipse Select the tool by clicking on it and then click on the spectrum to add annotation For example to add text select the Text annotation tool click on the spectrum where you wish to enter the text and then start typing the text To delete annotation double click on it to select it and then press the Delete key on the keyboard Tip To delete all annotations at once go into the context menu on the spectrum viewer Choose Select All from the Annotations menu and then select Delete from the Anno tations menu This operation will remove all the annotations from the current spec trum Show Data Values With this tool you can view the Energy keV and counts in any channel of the spectrum Simply select the Show Data Values tool from the toolbar and then hover on spectrum The values will be displayed as you move from channel to channel Show Candidate Elements Click on the question mark icon to select the Show Candidate Element tool Position the cur sor at the center of a peak by double clicking with the mouse Note you may wish to expand the spectrum horizontally by holding down the control key and dragging the spectrum with 175 the mouse The list of elements spectra corresponding to the energy at the cursor is dis pl
436. the mouse wheel to zoom in and out Fit to Height Adjusts the magnification of the pre view so that a single page fits within the full area of the window 50 Getting started The Business of Science Menu option Description Fit to Width Adjusts the magnification of the pre view so that the page fits the full width of the window Changing the logo in your reports A standard report typically contains a logo usually at the foot of the first page If you prefer to use your own logo you can replace the supplied logo To make this change you must have an administrator password 1 In the folder where you installed the software usually C Program Files find the file logo png in a subfolder called Reports 2 Open the file in a suitable graphic editor such as Microsoft Paint 3 Record the size of the original logo for example width x height 150 x 75 In Micro soft Paint this information is in Properties 4 In another folder create your own logo If your logo is smaller than the original logo surround your logo with white space to increase the image size Ifyour logo is larger surround it with white space to increase the image size and then crop the white space to create an image that has the same aspect ratio as the original image for example 400 x 200 5 Name your logo file as logo png and copy it into the installation folder You might be prompted for an administrator password
437. the six standard orientations and are a quick way of specifying the Specimen Orientation The lower seventh button allows the user to man ually type in a rotation in the numeric fields to the right When EBSD data Is rotated it is between two coordinate systems CS1 Data Acquisition Coor dinate system and CSO Sample Primary Coordinate system If the sample coordinate system and acquisition coordinate system are coincident then the default rotation will be 0 O 0 The data rotation is defined as the rotation from CSO to CS1 For example the rotation 90 90 90 means that the CSO coordinate system is related to CS1 in following way Y Ko Ko 90 90 90 Yo i CS0 Ji i Ko io The first angle is the rotation around the coordinate systems z axis the second angle is the rotation around the rotated x axis and the third angle is the rotation around the rotated z axis required in order to make the two coordinate systems coincide gt CS1 Li Note that the scanning system always has the x axis horizontal the y axis vertical and the z axis pointing out of the image so the orientation of the CS1 is always the same 415 Phases In order to index an EBSP the software needs to know what phase s is present in the spec imen This step provides the functions necessary to locate a phase in a database and add phases to the list of phases to include during acquisition Phases in Database You can select a database by using the d
438. the standards file The k ratios are then used in the Stratagem engine The nominal values specified in the sam ple model are used as the starting point of the true sample description The Stratagem engine then calculates what k ratios would be expected for this guess and compares these with the measured k ratios from spectrum processing It then refines the guess to forma new estimate of the true sample model This process proceeds by iteration until a sample model is achieved that is consistent with the measured k ratios The systematic errors between the predicted and measured values are shown as rel diff and these can be com pared with the statistical variation expected for the measured k ratios shown as rel sigma It is important that you review rel diff to see how good the fit is to the data If rel diff is high then the results should not be relied upon and you should consider ways to improve your results When the difference between the measured and predicted k ratio is greater than six times the rel sigma the relative difference will be displayed in red How large is the error of the result If the theory for X ray generation and the measurement of k ratios were perfect the reported values for layer thickness and element concentrations would give predicted k ratios that agreed with measured k ratios to within the statistical precision of the measurement The relative statistical precision is shown as re
439. then the slower the Phase ID process becomes For example if you have over 100 phases then it would be advisable to try and restrict your search criteria before indexing the EBSP You may check the Auto box which means that band detection and indexing will auto matically take place if you change any settings or adjust any of the parameters in the Phase Search Results list Alternatively you can manually detect and index the EBSP by pressing the respective buttons Since indexing is generally slower than normal because of the high number of phases it is advisable not to use Auto Suggested Settings Adjust the Maximum number of reflectors to a suitable value before indexing This value is dependent on the quality of the EBSP from the unknown phase but typically you may want to use more reflectors e g 75 100 than for normal EBSD analysis Note that increasing the maximum number of reflectors will also slow down the indexing process To optimize band detection it is recommended that you use a high Hough resolution for example 70 and a greater number of bands than for standard EBSD analysis If the EBSP has well defined sharp Kikuchi bands use the Band Edge detection Alternatively use Center detection Careful manual band detection is often the preferred method for accurate Phase ID It is advisable in the first instance to switch off the Advanced Fit mode The software will now try to index the EBSP using all of the possible phases y
440. this technique Press to display the results in a chart Spectrum 1 Spectrum 2 Br Weight o The sigma values are displayed as black or white vertical bands across the bars in the chart results as shown in the example above In this case the full scale of the bar chart is 50 If you wish to change the MiniQuant Settings press P All Elements Spectrum 1 Oxygen by Stoichiometry Spectrum 9 ee Element by Difference E Normalize Results o Apply 168 EDS SEM Oy 45O ND INSTRUMENTS The Business of Science Make your selection by clicking on the radio button and then press the Apply button The results will be updated immediately Note The Quant Settings in the MiniQuant and Calculate Composition are the same Updat ing one updates the other and vice versa 169 Confirm Elements athe Coni Elements This step has been designed to help you confirm the elements that have been identified by AutolD in your spectrum These elements are then used to create a confirmed elements list for qualitative and quantitative analyses Extensive tools including Element Series Markers Overlays Element Profiles and Show Candidate Elements are available here to assist you in confirming elements manually How to confirm elements Start with the largest peaks Press the question mark icon to select the Show Can didate Elements tool from the tool bar on the left han
441. this will affect where peaks appear in the spectrum The exact peak positions and the resolution of the system are needed to precisely identify individual peak components in the spectrum If peaks overlap the relative sizes of individual peaks can only be calculated accu rately if the width and position of each peak is accurately known By measuring the position of one known peak the system can be optimized to determine the position of all other peaks How often should I perform Energy Cal ibration The electronics used is carefully designed to provide good temperature stability Since a change of 10 C produces only a 1 eV shift in peak position most routine analysis can be per formed without re optimizing peak position However if you need the software to resolve very closely overlapped peaks you should perform Energy Calibration and re optimize if the ambient temperature changes by a few degrees With a good laboratory temperature control you may not need to optimize for many months How to perform Energy Calibration Energy Calibration requires the acquisition of a high quality spectrum from a suitable element from which details of the spectrometer gain are calculated and stored One element can be used for both the Energy Calibration and Beam Measurement or you can use two different elements if you wish You can use an element as an energy calibration standard as long as the calibration peak is not overlapped by other peaks Th
442. tion option is enabled by default and can be deactivate by un checking it in the Describe Specimen step as shown in the screen shot above You can then AutoID at any time by pressing the button Additional peaks in the spectrum can be identified manually by using the Show Candidate Elements tool in the Confirm Element step Click on the question mark icon to select the Show Candidate Element tool Position the cursor at the center of a peak by double clicking with the mouse The list of elements spectra corresponding to the energy at the cursor is dis played in the panel on the right By highlighting an element in this list you will see the markers showing all the lines for this element Note that the Identified Elements will be quantified if you have selected the Current Spec trum or the Fixed List and Current Spectrum Element List in the Quant Settings in the Cal culate Composition step or EDS Quant Settings in the User Profile dialog Note EDS Quant Settings are available in the User Profile Dialog accessed from the Tools menu These settings are also available from the Calculate Composition step Fixed List The elements in the Fixed List are defined in the Quant Settings dialog which is available in the User Profile and the Calculate Composition window Note that the Fixed List is only used for calculating composition in quantitative analysis Example I want to do quantitative analysis on my glass samples and want t
443. tion You can check the Fixed weight option and enter the value Deconvolution Elements Deconvolution elements may be used to select elements present in the spectrum that should not be quantified but whose influence needs to be accounted for when processing the spec tral data For example elements present in an oxidation layer or in a supporting grid If you wish to deconvolve elements from a spectrum select the required element from the drop down list and press Add element Further elements can be added or removed using Add element or Remove element respectively Selecting an element for deconvolution means the peaks will automatically be deconvolved from the spectrum but the element will normally not be quantified The deconvolution ele ment will only be quantified if it is oxygen and its composition is calculated by stoichiometry Ratio Standard A proportionality factor known as the k factor is used to relate the characteristic X ray inten sities 1A in a thin sample to the actual concentrations in wt in the form lt A Saga B where Intensity C concentration and K K factor K factors The k factor relates the intensity of two elements Where more than two elements are to be analyzed if all ratios are taken with respect to a single element this is called the ratio stand ard element these values can be regarded as elemental sensitivity factors more usually known as k factors The theoretical k factor va
444. tion areas to prevent them from overlapping and masking the text Shows the label for the image in the header Shows the Color Bar below the Image Viewer You can move the slider on the Color Bar to change the contrast of the image Shows a micron marker below the Image Viewer Shows the Auto and Manual buttons at the bottom right corner of the image Shows any annotations on the image Shows a color key of the phases in the bottom left part of the Layer Image in the Map application Smoothes the lines in the image If this check box is not selected the image might appear more pixilated If you save your project as an INCA project you can export a Secondary Electron SE or Back scattered electron BSE image Reports You can select the layout scale and content of your reports A report is typically a Microsoft Word document or a Microsoft Excel spreadsheet If you do not have those software appli cations installed you can still view and print the reports with the Microsoft viewers that are 18 Getting started The Business of Science supplied with the software To edit the reports you need Microsoft Office 2007 or later software installed on your computer Field Description Report Image Scaling Pix Sets the image scaling els Per Inch The default is 96 pixels per inch which is suitable for displaying ona computer screen For high quality printing select a higher number
445. tion toolbar These controls are at the top of the window above the electron image and the line scan Control Description Starts the acquisition of linescan data Stops the acquisition of linescan data w Opens a window where you can specify acquisition Settings l parameters such as the number of points along the line Offers a choice of processing Line TruLine or Quant Line LineScan viewer toolbar These controls are above and below the line scan Control Description li Changes the height of each element linescan in the Stacked view Offers a choice of display Stacked overlays multiple linescans in a sin gle view Vertical Tiles displays individual element linescans in a separate view You can change the height of each view using the Display slider bar Table displays data for each point and ele ment in a table layout 253 Control Description J Allows you to change the color and thickness of Settings l each line and the smoothing factor for all the linescans Extracts all spectra from the line Result Type Shows the percentages by weight or the number of atoms Available for QuantLine processing only Binning Factor Sets the binning factor Binning produces an aver aD aged signal which has less noise overall Acquire Line Data left toolbar These controls are at the top left side of the electron image Control Description Pans and
446. to Interactive and in a more com pact display Links images You can simultaneously manipulate all the layers using the pan or zoom controls Unlinks images You can manipulate individual layers using pan or zoom controls Use the mouse wheel to zoom in and out of the image Use these tools near the bottom right of the screen to adjust manual and automatic brightness contrast and color Context Menus Right click the electron image to display context menus for copying exporting and printing images See Also Scan Image Toolbar on page 424 Scan Image Settings on page 421 FSD diode controls on page 432 Context Menus Image Viewer on page 157 127 Export Settings on page 132 AutoLock on page 133 Scan Image Settings The selectable parameters that control image acquisition Image Scan Size Dwell Time and Number of Frames should be chosen according to your specific requirements Both the time taken and the data storage size of the image are dependent on these parameters For a quick look at the specimen select the lowest image scan size and the fastest speed This will enable you to decide whether you require either a higher pixel density in order to observe finer detail such as small features or a longer dwell time in order to improve the image quality by reducing the noise The available acquisition parameters are Image Scan Size Dwell Time us a Mains Synchronize Input Signal Softwar
447. to selection of number of bands It is easier to set up for data collection and to achieve a higher hit rate It is more effective at separating similar phases Band Width function replaced by Grouping Function accessed from the Describe Specimen Step See the links below for detail Optimize Solver on page 444 Configuring groups of phases on page 417 Magnetic Field Correction for EBSP s collected using SEMs with Immersion or Semi in Lens objective lens We now have the capability to correct EBSPs distorted by the magnetic field in the SEM chamber this method uses the model described in US Patent 2006 0219903 m This correction is designed to work on Hitachi and JEOL SEMs where the magnetic field is typically required for high resolution imaging Please check with OI to con firm that your instrument is supported XIV What s New in Version 2 0 The Business af Science The solution requires collection of a distorted and undistorted pattern from the same point and then calculates a correction factor See the link below for detail Magnetic Field Correction Setup on page 440 Forescatter Detector Control Improvements Additional functionality is included to aid the setting up and collection of FSD images There are 2 default settings a Atomic number contrast Orientation Contrast as well as a customized setting See the link below for detail FSD Control Dialog on page 434
448. to separate or resolve from another peak that may be close by in energy If Default is selected the Process Time is automatically set to a suitable value There is a trade off between the Process time that is used and the speed at which data can be acquired into the X ray spectrum Total counts in spectrum The default value for Total number of counts in spectrum is displayed here This value is used to acquire a spectrum before the Beam Calibration is performed You can enter the value that you wish to use The default value for the total number of counts is 600 000 It is the total number of counts in a Co spectrum acquired at 20 kV It gives an approximate precision of 1 in the value of beam current over a spread of 0 5 See Also Acquire Spectra Settings on page 313 71 In this section users are provided step by step advice on the most frequently performed tasks The following tasks are described in details EDS Qualitative Analysis 020 02222 c cece eee eee cece ee ee 73 aay es OXFORD J en INSTRUMENTS The Business of Science EDS Qualitative Analysis In EDS the qualitative analysis is the process of identifying elements present in a specimen It involves acquiring a spectrum from the specimen and then identifying the peaks in the spec trum Peaks can be manually identified to confirm elements using sophisticated tools avail able in the software Once you have identified all the
449. tom mode is described with screen shots here The four components in the Acquire and Confirm window are docked in the four quadrants of the work space as shown in the screen shot below iw p i e Suar Image acquisition al BS Spectrum acquisition application application sorai e PRT fis sega Spec OT gt Pe a i Se protie ae sl Sonn hj Electron Image 1 x 7 _ ue Be Confirm Elements a Quantitative analysis application application d Pe _ ue wos Step Notes S rouy V BPGWanaas TLALLLEL 1 Press al in the top left quadrant to undock the Acquire Image window The upper two quadrants are now filled with the Acquire Spectrum window 2 Click with the left mouse button in the title bar of the floating Acquire Image win dow and drag it to a second monitor Keep the spectrum acquisition window on the Primary Monitor 202 EDS SEM Oy 45O ND INSTRUMENTS The Business of Science 3 Toggle off the button in the toolbar near the top right of the main application to remove the Quant Results window from the display The Con firm Elements window will slide in under the Acquire Spectrum window as shown in the screen shot below The Spectrum acquisition Looban auet window occupies the top two from the display quadrants of the workspace i aa za 4 The Acquire Spectrum window can be removed from the display if you need to max imize the Confirm Elements disp
450. tween the reference images The Predictive correction will be updated when a tracking image is acquired FAQs about AutoLock AutoLock is designed to aid in the stability of data acquisition on SEMs and TEMs where the image may shift This image shift can occur for a number of reasons such as sample move ment due to temperature changes at high magnifications or charging of the sample AutoLock works by acquiring an image comparing it with a reference image acquired from the same area and determining the image shift The scan position is then adjusted to com pensate for the shift 140 OXFORD E en INSTRUMENTS The Business of Science What is the difference between Reactive and Predictive Drift Correction There are 2 modes of AutoLock operation Reactive Drift Correction It collects an image after a certain time lag This time can be manually set or automatically cal culated This image is compared to the original reference image and the drift between the two images is measured If there is a drift between the two images then beam shift is used to correct it Reactive drift correction can be used independently or can be combined with Predictive Drift Correction Predictive Drift Correction It applies a linear extrapolation taken from the last two drift measurements over time It con tinues to correct until the next full drift measurement Predictive correction requires two ini tial reference frames which are acquired
451. u have stored EBSPs without solving Details opens the dialog showing EBSD Data Details AQ eo O RD Getting started INSTRUMENTS The Business of Science Each map components Band Contrast Phase Color Eulor Color IPF X IPF Y and IPF Z has six menu items m Rename this renames the selected component Delete this deletes the selected component Save As this saves the selected component as an image file Print prints the selected component Email sends the selected components via email Details opens the dialog showing details of the selected component Point Data There are two menu items for the Point Data Rename and Delete EBSD Point n There are six menu items for each EBSD Point as in the case of each map component described earlier Spectrum n There are six menu items for each Spectrum as in the case of each map component Mini View The Mini View is an area of the Support Panel dedicated to the display of a number of dif ferent views which you can select depending on what data you wish to view Views con taining the current Electron Image Spectrum Monitor or EDS Ratemeter are examples of such views Electron Image The full field of view of the currently selected electron image is displayed here It is often use ful to refer to this image in steps where your application area is dedicated to displaying spec tra or maps For example you can view the electron image in
452. u wish to view full size spectrum in the Acquire Spectra step The features of the electron image in the Mini View are The default state is full image with Scale Bar micron marker You can remove the Scale Bar from the display by de selecting it from the image context menu The Context menu items are 93 Show Acquisition Areas Show All Show Selected Show None Show Scale Bar Features such as Pan Zoom and User Annotations are not available in the Mini View Spectrum Monitor It provide a means for the user to see what X rays are being detected at any given moment It is useful for a quick survey of the specimen to find an area of interest for analysis Spectrum Monitor uses the current spectrum acquisition settings with the additional setting of the refresh rate for monitoring the spectrum This refresh time is referred to as the Buffer Size The default is 20 but can be changed under the Settings for Soectrum Monitor in the Mini view Increasing the Buffer Size corresponds to a longer refresh rate The settings in the Spectrum Monitor are Buffer Size The default value is 20 Number of Channels 1024 2048 or 4096 Energy Range keV 0 10 0 20 or 0 40 The settings can be selected from the Acquire Spectrum step or Mini View If you make a change in the setting in one place it is automatically updated in the other Ratemeter It is very useful for setting up the microscope beam current while viewing the X ray acqui
453. ue to temperature changes at high magnifications or charging of the sample AutoLock works by acquiring an image comparing it with the reference image acquired at that Site determining the image shift and adjusting the scan position to compensate for the 133 shift AutoLock will correct for an image shift at the interval specified while acquisition is in progress Note AutoLock is accessed from the Settings in the Scan Image step in the Guided mode and Acquire and Confirm step in the Custom mode of Point and ID navigator In Map and Linescan AutoLock is accessed from the Settings in the Scan Image step in the Guided mode and Acquire and Construct step in the Custom mode To display the status of AutoLock in the Status Bar On Off Due Acquiring check the AutoLock Status check box in the Status Bar tab in the Preferences dialog You can access Preferences from the Tools menu Setting up the AutoLock 1 Enable the AutoLock from the Settings in the Scan Image screen Set it to Auto or Custom mode using the appropriate button There are three modes Off Press the Off button to disable AutoLock Auto In the Auto mode the system chooses a set of default settings This would typically use a 50 reduced scan at low resolution providing AutoLock for a distance of half the scan area If you require extra correction use the Custom setting The tracking image settings are displayed but the Scan Settings and Predictive Settings
454. uisition toolbar and other nearby controls The acquisition toolbar above the electron image and below the Navigator has buttons for starting and stopping the image acquisition the Settings cog for selecting the image acqui sition parameters and a button to link unlink images for manipulation oe New Site Scan Image gt STAR 8 STOP Settings Select Second image None DE g g g 125 Control Description Displays up to three combinations of mixed image and ai individual images Your selections are retained in your FSD only user profile gt START Click to start the image acquisition according to the cur rent acquisition parameters Click to stop image acquisition Acquisition stops at the end of the current frame Click again to stop imme diately If you navigate away from the step acquisition stops at the end of the current frame To change the acquisition parameters click the Settings cog on the Acquisition Toolbar to display a dialog You can select Image Scan Size Dwell Time us Input Signal the labels here reflect whatever was set during the installation for example SE BSE or FSD either Con tinuous Scan or Number of Frames and Frame Time secs If your specimen is drifting you can activate AutoLock to ensure that any analysis corresponds to the true loca tion on your image Mixing Mode Combines signals from the diodes to form a mixed image Some options are available only if the requir
455. ul shortcut menus available as right mouse click in the spectrum viewer are shown in the table below Context Menu Item Reset Scales Export Peak Labels Annotations Save As EMSA Copy Print Email Settings Show Reset Posi tions Show Select All Style Delete Show 103 104 Context Menu Item Locked This is a useful option if you are looking for a particular energy range You do not want the energy scale to change when you load a new spectrum In the viewer for exam Ination or for report ing Locking the X Axis will main tain the hor izontal energy scale If you do not lock it it will change to the full scale when you load a different spectrum The default energy range Is full scale Adjust EDS SEM The Business of Science Menu Item Show Locked 105 106 Context Menu Item Units You cps eV have the choice between cps eV per channel and Counts for the units along the Y Axis of the spectrum For easy comparison of spectra cps eV is an ideal choice because there is very small var lation in the range You do not need to nor malize prior to com parison of spectra using dif ferent energy ranges number of channels and live times This is vital when comparing a stored spectrum with one that is still EDS SEM The Business of Science Menu Item acquiring
456. um The number of eV channel will depend on both the energy range and the number of channels you select Energy Range keV Number of Channels eV channel In the Auto mode the system checks for the energy range selected and sets the appropriate number of channels Note The Energy Calibration routine is performed for all process times and for all available energy ranges and number of channels It means if you change any of these settings soon after you had performed the Energy Calibration you do not need to re optimize the system Process Time Select the Process Time from the drop down list of Process Times Default and 1 to 6 The Proc ess time Is the length of time spent reducing noise from the X ray signal coming from the ED detector during processing By selecting different Process times it is possible to reduce dif fering amounts of noise The longer the Process time the lower the noise If noise is 97 minimized the resolution of the peak displayed in the spectrum is improved in other words the peak is narrower and it becomes easier to separate or resolve from another peak that may be close by in energy If Default is selected the Process Time is automatically set to a suitable value There is a trade off between the Process time that is used and the speed at which data can be acquired into the X ray spectrum Process time 1 is the shortest and as such gives the highest X ray acquisition rates but at some cost to
457. unknowns that produce an iden tical set of line intensities in which case the problem is unsolvable under these conditions The Calculate Solubility tool takes all this into consideration and will work out those kV ranges where the problem is solvable and those where it is unsolvable It also takes into account how the intensity of lines varies with kV and will calculate the relative statistical var lation in all the determined unknowns so that a figure of merit can be plotted as a function of kV The kV at which the problem is solvable is marked in green and where it is unsolvable is marked in red The Calculate Solubility tool will try to find a kV where the problem is both solvable and where best precision is achieved for the unknowns to be determined At this kV the tool will show the best X ray lines to use for the analysis If you are an expert this choice can be over ridden Furthermore an expert can over ride the default choice of allowed lines that the Calculate Sol ubility algorithm is allowed to use for each element However in most cases this intervention will not be necessary If you want to find out exactly what sort of precision can be expected from the analysis there is a Simulation tool that synthesizes the spectrum that would be achieved in real life on the microscope If the simulated spectrum is then analyzed you can see what sorts of results are generated and what precision is achieved in the unknown variables If the p
458. uous Scan 421 Number of Frames Frame Time secs FSD Control m AutoLock Image Scan Size In general the resolution of an image or Image Scan Size is defined as the number of picture points or pixels along the x and y axes e g 256 x 256 512 x 512 or 1024 X 1024 The quality of the image improves as the resolution at which an image is acquired is increased However a microscope monitor CRT is usually a rectangular display rather than square so the res olution is displayed as a rectangle i e 256 x 200 in order to take into account the aspect ratio The y dimension is set at installation when imaging is calibrated It will vary with each system Select the Image Scan Size for image acquisition from the following drop down options avail able 64 128 256 512 1024 2048 4096 8192 Dwell Time ps Images can be acquired using different speeds The beam dwells on each pixel for a specified length of time while the signal is collected and then it moves to the next pixel So the speed at which an image is acquired depends on the dwell time Speed Dwell time Fastest Fast Normal Medium Slow Slowest Mains Synchronize Selecting Mains Synchronize on the Image Setup window synchronizes the start of each scanned line to the mains supply This will help to reduce mains borne interference in the image Note that the acquisition time will be marginally longer than when mains synchronize is not selected
459. used for the phase search process however it requires that the databases are first copied into the C CHANNELS directory See Also Confirm Elements Settings on page 171 Confirm Elements Tools on page 174 Element Lists on page 191 Peak Labels on page 158 Compare Spectra amp MiniQuant Results on page 195 Quant Settings on page 187 479 Identify Phase The purpose of this step is to use the phases in the Phase Search Results area to index the EBSP shown in the image viewer and display the solution s The phase that gives the best solution to the EBSP can then be manually added to the list of phases for acquisition This phase is then available to use for example during mapping Phase Search Results This list of phases comes from the spectrum and is generated from the previous step You can now prepare it for indexing The list of phases together with the number of reflectors and phase color is shown in this table You may wish to review the details of a particular phase To do this highlight the phase from the list and select the tab you wish to use from the Phase viewer below Phase Color The colors for the phases are picked automatically with the same color being used for the phase as used in the 3D Phase View and the simulation used on the EBSP You can manually change the color if you wish but the software will attempt to pick a unique color for each phase Maximum reflectors Rather than having to
460. using the Pan or Zoom control Press trol to unlink images You can manipulate individual layers using Pan or Zoom con Brightness and Contrast You can adjust the brightness and contrast of the currently selected image or map Press on the Display toolbar to open the Brightness and Contrast dialog 209 Auto Brightness and Auto Gamma Using the Auto brightness and Gamma buttons on the bottom right hand corner of the Map display window allows you to change the Brightness Contrast and Gamma for all the maps The Auto Brightness button optimizes the maps to give the best Layered Image and the Auto Gamma enables you to see all the map data including background noise Element Maps View Settings You can manipulate and view the data by using various parameters available in the Settings H Settings Sort Order Maximum intensity Layer Visibility Selection Q Manual Auto maximum intensity Smoothing Level 1 NoSmocthing Ei ACB while acquiring Sort Order There are three different ways of sorting maps Alphabetically By atomic number By maximum intensity in map sorts on the value of the brightest pixel in cps Layer Visibility Selection You can choose how the visibility of layers selected in the layered image There are two options Manual and Automatic In the Manual mode you must select which X ray maps to be included in the layered image In the Automatic mode first N maps Number of
461. veeved 6 Preference 2 22 cece cece eee eee eee cece eee eee cece cece eee eee eeeeeeeeeseeeeees 13 SILLTE gt AE E E E EE EEA EE O EEEE E 20 User Profile 0a0a0000a0a0a000a0a 0000000000000000 0000000000 a000 000a 0 oaaao ooroo 22 Support Panel 2 000000000000 0000000 000000000000000 0000000000000000 202a oaoa oaran 27 Report Results 22 002 2c icc ec eececccc ee ccc cece cece cece eee eeeeceeeeeceeeceeeeeeees 44 Tenes aeee aston ce ee ae adres bat vena ae teen aterotaceeieasanedsctee 53 aA ee Waa en en ne nO COD Oe Se eee ne 54 Color KEY nae ne A E ee ee eee eer 55 FAQs about Software Licensing 22222 c cece eee ee eee cece ee ee eee cece annann 56 Moving data to another PC 2 2 cece eee eeee ees 59 Getting LOU iirc dca eee ade doi Sescwneeeaateeayeeuccadeecde nononono onenera 61 eS SI cis ee ce a ee ee 63 Set p for ioscan es ek ose 65 CAUDA ea ee ence on E ee ete cue een cee ca anece ensue E A 66 Calibration Element 0 000022 c cece cece cee cece ee ee eee eee cece cece eeeees 70 Calibrate for Beam Measurement Settings 00 2 2222 e cece eee ee eee eee eee eee 71 POW UO vy cette hence ee tetas rnc wee ota senna eens Loe aeeaasudeenbeakueouaunnce 72 EDS Qualitative Analysis 000 0 22222 c eee cece cee eee ee eee e eee eee ee cee eee eee 73 Analyzer Guided __ 2 2222 o oie eee c cc eeeeneeeeeeecen eee rannen 75 DESCrIDE SUCCING Rica doves eee eee nett Jdeewaceceensenut
462. vetime and analysis lines to be used for subsequent acquisition of spectra from a particular type of sample To use LayerProbe you need to be able to define which elements exist in each layer their approximate concentrations and the order and approximate thicknesses of the layers You can then select which thicknesses and concentrations you want to determine unknowns and define those you already know fixed variables It is also necessary to define the X ray lines to be measured and which acceleration voltage kV to use The choice of X ray lines and kV will depend on the problem to be solved and that requires expert judgment LayerProbe includes an automatic tool Calculate Solubility which helps to find the best lines and kV to use for a particular problem The tool will look at what you wish to determine unknowns and what you do know fixed variables and will scan a range of kVs trying to find a kV where the problem can be solved LayerProbe has to determine all the unknowns you have asked for by measuring the X ray line intensities for the elements present If more unknowns are to be determined than there are lines available the problem will be unsolvable It can be more complicated than that because at different kV different lines K L M are excited the electron beam may not pen etrate all the layers and some X ray lines may be absorbed on their way out to the detector Furthermore sometimes there are various combinations of
463. ways 100 Setting an element to difference can be used when analyzing a specimen in which a sig nificant quantity of a light element which cannot be detected but is known to be present It can also be used in cases where an element is present for which no standard is available Unknown If the element is defined as Unknown the concentration entered will be used as a starting value for the model refinement in the calculation The closer this estimate is to the real composition the quicker the LayerProbe calculation engine will be to achieving a result A layer must have two or more unknown elements to use the Unknown concentration option Note that if there is only one element in a layer then this must be defined as Fixed and the concentration must be entered as 100 Wt 3 Defining the density of each layer Ifyou know the density of a layer enter it in the Density text box It is expressed in g cm3 Note that when a composition containing a single element is entered the density is auto matically set to the element density Internally LayerProbe calculates the mass thickness of each layer The mass thickness is defined as the product of the density of the material and its thickness Hence to determine the thickness the density of a layer must be known and be entered into the model Therefore it is important to realise that the accuracy of the value in density directly affects the measured thickness 4 Defini
464. when a spectrum has been quantified 307 Calibration Element Select the element that you wish to use for Energy calibration from the drop down list The elements available for Energy Calibration are tabulated below X ray peaks often involve multiple lines and in order to achieve accurate calibration a large peak with well known line energies and intensities is required Therefore for this reason we recommend that for energy calibration a pure element is used If a pure element is not available compounds that have K lines that are not overlapped may be used instead However there may be some loss of accuracy because the line energy in a compound can sometimes be up to 2eV different from that in the pure element 308 EDS TEM The Business of Science Analyzer Guided There are two modes of operation in the Analyzer application Guided and Custom In the Guided mode the Analyzer navigator has five following steps Describe Specimen 2 0022 c eee cece cece cece cece eee eeeeee 310 Acquire Spectra 22 22 0000 2 22 cee cece cece ee cece cece eee e eee eens 313 Confirm Elements 22 22 2222 e cece cece cece ec ceeecceeeeceeeees 330 Calculate Composition 0 000 222 c cee cece cee eee ee cece eee ee 332 Compare Spectra 2 2 22 2 ee eee 338 309 Describe Specimen A Describe Specimen In this step there are two tabs Su
465. y Range keV Select a spectrum energy range from the available options of Auto 0 10 0 20 or 0 40 keV from the Energy Range drop down list 313 An appropriate energy range should be selected in conjunction with the current microscope accelerating voltage If the accelerating voltage is above 10 kV in order to view lines which may be excited above 10 keV the 20 keV range should be chosen Below 10 kV it may be more appropriate to choose the 10 keV range since no lines above 10 keV will be excited In the Auto mode the system checks for the accelerating voltage set on the microscope and selects a suitable energy range in the software Number of Channels Select number of channels from the drop down list of Auto 1024 2048 or 4096 4K with which you wish to display the spectrum The number of eV channel will depend on both the energy range and the number of channels you select Energy Range keV Number of Channels eV channel In the Auto mode the system checks for the energy range selected and sets the appropriate number of channels Note The Energy Calibration routine is performed for all process times and for all available energy ranges and number of channels It means if you change any of these settings soon after you had performed the Energy Calibration you do not need to re optimize the system Process Time Select the Process Time from the drop down list of Process Times Default and 1 to 6 The Proc ess time i
466. y inserted the detector will be retracted Allow Movement This is the default state It is shown when no interlocking takes place because no inter lock is configured or because the interlock allows the detector to be moved Prevent Movement This state appears only if the interlock is con figured and the SEM is in a state in which the interlock does not allow the detector to be inserted Detector Positioning The buttons on the Position tab control the movement of the detector Starts moving the detector into the chamber until either the movement is stopped by the operator or the detec tor reaches its fully inserted position 491 Button Description Starts moving the detector out of the chamber until the movement is stopped by the operator or the detector reaches its fully retracted position Stops the detector move ment immediately at any time Move To Moves the detector to a spe cific position Type the inser tion distance in the box to the right then click Move To Step In Step Out Moves the detector a fixed distance inwards or out wards Type the distance in the box to the right then click Step In or Step Out to move the detector by the required distance 492 Hardware Control OXF INSTRUMENTS The Business af Science Microscope Control The Microscope Control application is provided for controlling and reading the microscope i TI parameters When
467. y peaks often involve multiple lines and in order to achieve accurate calibration a large peak with well known line energies and intensities is required Therefore for this reason we recommend that for energy calibration a pure element is used If a pure element is not available compounds that have K lines that are not overlapped may be used instead However there may be some loss of accuracy because the line energy in a compound can sometimes be up to 2eV different from that in the pure element For Beam Measurement The system standards were calibrated using Co as the beam measurement element Pure Co resists oxidation and polishes well and is therefore the most suitable choice to monitor beam current when you want to obtain accurate un normalized or absolute estimates of com position However below 15kV Co K is weakly excited and it is preferable to choose another pure element for monitoring The system will then make suitable corrections to allow the fol lowing pure elements to be used If the beam measurement standard is oxidized contaminated or has a rough surface then this will have a direct effect on analysis totals 70 EDS SEM The Business of Science Calibrate for Beam Measurement Settings When you select Beam Measurement the Settings icon is enabled These are the same X ray acquisition parameters which you have selected in the Acquire Spectra step You can change the settings here if you wish The paramete
468. y points along the line To pre vent an excessive amount of data you can apply a binning factor to limit the number of points 1 Click the Extract Spectra button below the linescans 2 In the Reconstruct Spectra dialog select a binning factor 3 Click START to extract the spectra for the points into the project The data is saved in the Data Tree with this icon See Also How binning affects the quality of your data on page 373 Acquire Line Data Settings A settings cog in the Acquire Line Data window provides access to the settings for acquiring linescans G Settings Acquisition Time Until Stopped Fixed Duration Number of Passes 2 Number of Channel Auto Energy Range keV Auto Process Time Default Pixel Dwell Time ms 5 Number of Points Pass Live Time s You can specify the Acquisition Time Energy Range keV Number of Channels Process Time Pixel Dwell Time ms Number of Points in the line or the separation between points and Live Time s per Pass 252 EDS SEM The Business of Science In the Auto mode the system checks for the accelerating voltage selected on the microscope and sets the appropriate spectrum Energy Range Based on the Energy Range selected an appropriate value for the Number of Channels is set automatically Use the Default Process Time if you wish to acquire good quality data at the optimum speed Toolbars Acquire Line Data Acquisi
469. yer modes legend on images images explaining the colors on license linescans acquiring averaging comparing elements on displaying distance between two points element counts and percentages exporting data in Data Tree manipulating shortended by binning smoothing speadsheet toolbar logo change in reports Index 432 431 426 129 131 423 425 431 430 429 61 54 426 18 469 469 216 55 56 241 391 248 398 247 397 243 393 245 395 246 396 250 400 249 399 243 393 215 224 373 248 398 250 400 253 254 51 501 magnetic field correction Magnification map area calculator maps effect of binning layers menu bar menus Data Tree File Tools View Microscope Control Mini View mix layer mode N noise peak excluding when resetting scales setting cut off voltage noise reduced by binning Normalize O oimfc file magnetic field correction oip file Orientation information orientation pole figure overlay layer mode P pan on electron image peak identification peaks no label in spectrum no low energy noise 502 440 31 87 493 496 450 214 224 373 216 6 38 7 10 9 493 41 93 216 101 102 102 214 223 373 2 100 120 152 174 188 247 317 338 358 397 440 59 465 468 216 131 424 66 101 102 101 Index The Business af Science Phase Image data tree 33 89 phase maps i
470. ys tem The name of the folder is the same as the Project name The Project folder contains a sin gle file with an oip extension and optional Data and Reports sub folders Note When moving or copying project data ensure that the root project folder is moved copied not just the oip file The folder can be zipped using the standard 30 Getting started O45 O ND INSTRUMENTS The Business af science Windows compression utilities if required Specimen Specimen represents the real specimen that you analyze and collect the data from including images maps and spectra There may be many Specimens in a single Project A Specimen may contain more than one Site ca Site Site represents an area on the Specimen from where you acquire data such as images spec tra and maps Site can hold multiple images for example SE and BSE plus any imported images The analytical conditions such as kV Magnification and Calibration are stored with the data Electron Image Electron Image on each Site can be a secondary electron SE image a backscattered electron BSE image or a forward scattered electron image You can acquire two images simul taneously if suitable hardware is available FSD Data This folder is the container for all FSD data It contains electron images from each diode and the FSD mixed image which is the result of combining some or all of the FSE images FSD Data 2 Folder of images J F
471. zooms the image or linescan Adds annotation to the image The caliper tool measures distances between points on the image and the linescan Marks the line on the sample then acquires the data Extracts a spectrum from a point on the linescan Shows intensity at any point on the electron image Shows the counts per second or element percentage on each linescan See Also Acquiring linescans on page 391 Acquire Line Data Settings on page 252 254 EDS SEM OXFORD INSTRUMENTS The Business of Science Construct Linescans S _ Construct Linescans In this step you can define energy windows and configure X ray line series to update the dis play of element linescans in the viewer You can use AutolD for initial display and then add or remove elements as you wish using the periodic table and the controls available in the Linescan Details dialog Linescan Details seyd uawa paalas Indude i E Clear Al In addition you can view the Line Sum Spectrum and navigate to the Confirm Elements step from within the Construct Linescan step to manually confirm elements 2595 Te aa Line Sum Spectrum 4 Fe Fe Ti 2 4 6 keV Manual selection of energy windows and X ray lines 1 Press to open the Selected Elements Details dialog Selected Element Details Element Beryllium Label Energy Window Selection Automatic Specify Line

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