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Iridium Ultra Version 1.4 Software User`s Guide

1. Selecting View Overlay Elements from the menu the following panel appears Selecting from the list of Elements on the left of the panel and clicking on one of the following buttons will overlay elements et This button adds the selected element to the Composite The color used for the element is the next default color available There are three default colors Red Green and Blue They are selected in that order When all three default colors have been used in the Composite only the gt gt Coler button described below can be used to add more elements Color HES Basic colors gt gt Coler Lele This button adds the selected element to the Composite using _ et any color The following standard Windows color selection dialog will Er Tl SE appear Select a color for the element using this dialog am e m A E E E E o Eee eee The button is used to remove an element from the Composite le E Select an element from the Composite list and then click this button to E EE remove it ree ne a a a Each element in the Composite has a threshold The threshold selects a E M minimum x ray count in the map for display of a pixel from the element Define Custom Colors gt gt A common use of threshold is to determine a background level for an Cancel element By default the threshold is set to 0 which will overlay any intensity from the element on the Composite By increasing the threshold for an elem
2. B Ne a 0 e as Se Cursor Vert 327075 Sami 9 8 2 Locations Menu The locations menu at the top of the panel can be used to print the locations list copy it to the Windows clipboard or export it to TAB delimited text file f Sample 7 Element Intensi Locations Sample 7 Element Intensities Concentrati mn Locations Intensity Concentration Show Spectrum Locations Mode Selecting Concentration OF hin SEE ie in the panel will apply Location Fe C Spat Spot Size Save Spot i 53 8047 ZAF corrections to the i ana west ct intensities and re display Rectangle H ca T Pai the histogram with these er aoe calculated values in weight percent as shown The Locations list will also display concentrations me i ull 1 107 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 9 9 Overlaying X ray Maps Composites X ray maps can be overlaid to reveal relationships of combinations of elements and the SEM image The map formed by overlaying the elements is referred to as a Composite map Below is an example of Fe and C overlaid on the SEM image i X ray Map Element Intensity Overlay SEM C Fe lt Composite Overay Settings Element Threshold Filters Iransparency SEM WA None 4 La t F Smooth 11 Median Fiter 2 Epot To Clipboard Auto Level after Filter
3. Monake IXRF Coleen ZD N es To access the color preferences select Properties from the menu and click on the Display tab as shown Then click on the Display and Print Settings button The Spectrum Display panel will appear as shown below ausam ert Bae EEE Hae Ze Bee DE EE OMN BiN The Display Colors are for the screen and the Printing Colors are for printing exporting and copying to the clipboard Checking the Transparent Background box means that the background will be left blank during printing Color selections in this dialog are done with the standard Windows color selection dialog as shown The color can be selected from one of the basic colors or a custom color can be defined and selected Status Information enables the printing of the cursor status information below the spectrum When enabled all of the cursor status information as displayed on the screen is printed When disabled this information is not printed Show MLK Buttons enables the display of the MLK buttons below the spectrum When enabled buttons appear under the spectrum at the location of the Ka line for as many elements as is possible to fit on the screen 31 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 Vertical and Horizontal Grids displays grid lines on the spectrum This is selectable separately for the display and printing Vertical Scale displays a vertical scale in counts on the left edge of
4. Sum Spectrum S 10 2 ol mel bd Ce LA lel El lel d el d el be El fel i The Maximum Pixel Spectrum is calculated and displayed with the menu item Process Maximum Pixel Spectrum It can be used to detects elements that are only present in a few pixels in the map The Maximum Pixel Spectrum is a spectrum comprised of the maximum x ray intensity from all pixels in the map For example the intensity in the spectrum at 6 4 keV is the maximum intensity found at 6 4 keV from all of the pixels in the map This pseudo spectrum has the principal characteristics of a real spectrum so that x ray peaks corresponding to highly localized trace constituents or foreign contaminants even those that are confined to one pixel of the image can be seen at a glance Below is an example of a Maximum Pixel Spectrum Sum Spectrum Maximum Pixel Spectrum 10 HOA fF Oe e ee oe Cursor 3 550 keV 4 cnt ID Pdlg2 Pdlg3 U mgl In b4 Pu mb Cd b2 In b3 At mln U mg2 Vert 50 Window 0 010 40 950 2796 cnt lt gt 103 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 9 6 1 Element Selection Both Sum Spectrum and Maximum Pixel Spectrum can be used to directly add or remove element maps to the display All of the manual peak identification techniques used on these spectra will invoke a feature to add remove the selected element For example clicking an element label button below the spectrum or using the Periodic Chart tool of
5. The ratio of the integrals is used as a scaling factor that is applied to all the channels of the match spectrum 3 Achannel by channel chi square fit is calculated over the Fit Region as defined in the Match Setup 4 The chi square fit is kept in an ordered list of best matching spectra The 10 best matching smallest chi square are kept for later viewing 4 14 1 Qualitative Match Analysis To setup an analysis using qualitative match the following steps need to be done e Acquire and save spectra from the materials for which you will be doing the match analysis These spectra should be stored in a unique directory apart from all other spectra The reason for this is that the match analysis will compare all match spectra in the specified directories see Match Setup below against the sample spectrum For example if you have a set of steel spectra that you wish to use for match analysis it would be appropriate to create a new directory on your computer named STEELS and store these spectra in this directory This directory should only be used to store steel spectra that you wish to compare sample spectra against e Setup an Analysis Settings file with the Quantitative method set to Match This is done by setting the quantitative method for all elements to be Match select Match as the quantitative method on 67 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 the Quantitation tab of the Spectr Properties IXRF Calib
6. then right click over the SEM spectrum and select Acquire from the menu To acquire the XRF spectrum make sure that the SEM beam is turned off then right click over the XRF spectrum and select Acquire from the menu 7 2 Identifying Peaks Use the same tools for identifying peaks on these spectra as you use with other spectra The only difference in the tools is that you must use the right click menu on the spectra to view the Periodic Chart View Periodic Chart Elements identified in one spectrum are automatically added to the other spectrum however the MLK markers are not automatically displayed on the other spectrum 7 3 Quantifying Spectra The Combined SEM XREF quantitation has 3 unique quantitative methods These are e Auto Uses ZAF and FP methods selecting automatically which to use e LS SEM Uses a Least Squares calibration file applied to the SEM spectrum e LS XRF Uses a Least Squares calibration file applied to the XRF spectrum To set the quantitation method right click on the spectrum and select Properties from the menu Click on the Quantitation tab and a panel similar to the following will appear In the Quantitation section select Method A panel similar to the following will appear Of course if you want to quantify specific elements with ZAF or FP this is always available Clicking on the Advanced tab on the spectrum Quantitation panel shown above will allow you to change individual element quantitat
7. Detector Parameters Detector Type This is the type of detector installed on the system There are three types User Defined SDD and Si Li The SDD and Si Li selections are pre defined typical detector settings User Defined does not have any definite settings the user must enter all pertinent settings Detector Element This is the material element from which the detector crystal is made Itis normally Si for the standard Si Li detectors the Li concentration is negligible Detector Area 58 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 This is the active area in square mm of the detector crystal Note that the active area maybe less than the area of the whole crystal which is usually collimated to only accept x rays in the center area where the peak resolution is usually the best Detector Collimator This is the diameter in mm of the collimator placed in front of the detector crystal as described above Detector Thickness This is the average effective thickness in mm of the detector crystal within the active area For Si Li detectors this value is almost the same as the actual physical thickness but for some thin detectors e g Si drift or pin diode detectors it may be significantly less because a significant fraction of the detector is not fully active Dead Layer Thickness During the processing of detectors e g the manufacture of Si Li detectors by the so called Li d
8. Es Fm Note that this procedure is unlikely to be completely accurate and the analyst should either confirm the results manually or severely constrain the list of likely elements to Keep Element List for Next Spectrum be present Also note that any shift in the peaks mis calibrated energies will result in a less accurate ID analysis 4 7 7 Configuring Automatic Identification Automatic peak identification operates on the original spectrum and works best when it has been optimized Automatic peak identification is configured on the Element ID tab of the Spectrum properties Select Properties from the spectrum s menu and then click on the Element ID tab as shown Save Settings Set As Defautt Apply To 35 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 Click on the Setup button to configure automatic identification A Daatomaholicnahcanal Setup panel similar to the following will appear View ID Details Peak Sensitivity 2 0 The parameters that are used to optimize the Automatic peak identification are Soa eee ee Peak Sensitivity During the first part of automatic element identification peaks in the spectrum are located Increasing values make the automatic identification more sensitive including smaller peaks in the identification process The default is 2 Search Width After the peaks in the spectrum have been located element lines are associated with each peak For a
9. Homegroup es Network al Adobe RoboHelp 7 What do you want to do W ork with A may Mans Work with X ray Line scans Double clicking over the Sample Name on the status bar will display the panel for editing the Sample Name just as the File Set Sample Name menu item does 14 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 3 4 5 Image Browse Displays images as thumbnails Click on Select Folder to change the folder from which images are displayed Click on an image to select it 10000rmaq 100maqg 3 4 6 Image Batch Export Exports multiple Image files automatically Image Batch Export Look in G IMRFDATA be My Computer TT My Network Files of type Image im Cancel Places File name t Help With Annotations Export Image File Format PEGE ipal Save ln Select one or more image files use the shift key to select multiple files Select With Annotations to include the annotations on the images e g magnification micron scale bar any annotations such as text drawing objects etc Choose the Export Image File Format and the folder in which the exported images will be Saved In 15 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 3 4 7 Setup Export Formats Allows for selection of image file formats for the export panels Throughout the software there are options to save data in a graphic image file format such
10. Palettes plt Open as read only 7 gt Name Date modified _ DEFPAL1 PLT _ DEFPAL2 PLT _ DEFPAL3 PLT _ DEFPAL4 PLT _ DEFPALS PLT _ DEFPAL6 PLT 2 23 2011 2 33 PM 1 6 1996 5 14 AM 4 7 2003 8 59 AM 1 6 1996 5 14 AM 1 6 1996 5 14 AM 1 6 1996 5 16 AM 1 6 1996 5 20 AM 1 6 1996 5 19 AM 2 23 2011 2 33 PM 1 6 1996 5 14 AM 4 7 2003 8 59 AM PLT Fil PLT Fil PLT Fil PLT Fil PLT Fil _ To replace one of the default palette files with the present color palette click on the Save File button A dialog similar to the following will appear Save in di Palettes _ DEFPAL2 PLT _ DEFPAL3 PLT _ DEFPAL4 PLT _ DEFPALS PLT _ DEFPAL6 PLT _ DEFPAL PLT _ DEFPAL8 PLT _ defpala plt __ defpall0 plt _ defpall1 plt _ defpall2 plt _ defoall3 olt Select the color palette file that you wish to replace from the list and click on the Save button File name ph Save as type 9 3 2 Setup Palette Files By default the palette files are assigned to elements in sequential order e g defpall defpal2 defpal3 as elements are added to the map Using the Setup Palettes panel allows for assigning a specific color palette to an element To access the Setup Palettes panel click on Setup Palettes on the Element Selection tab of the Properties panel as shown A panel similar to the following will appear 100 L SEM Palette e m Date modified 1 6 1996 5 14 AM 4 7 20
11. With X ray Maps X ray maps are excellent tools for determining the location of phases particles and other features on a sample that can be discriminated by variations in elemental composition An x ray map is performed by rastering the microscope s beam over the sample The scan area of the beam is divided into a rectangular grid of pixels The beam is then sequentially positioned on each of these pixels and x rays are acquired The x rays are displayed on the screen as rectangular images maps one for each element in the element list for the map The maps display as gray level images The map for an element visually depicts the number of x rays for the element at each pixel As an example this x ray map displays the distribution of elements in a ceramic sample Our software provides an advanced type of X ray map which is called FastMap FastMaps acquire and display the x ray maps for the elements in the element list and also store information that allow for viewing the full spectrum from each pixel Below are the advanced features of the FastMap Ability to view total spectrum from the x ray map Ability to view the spectrum from each pixel in the map Display a map for any additional elements desired without re acquiring the x ray map FastMaps can be saved with or without the spectral data When stored with the spectral data all of the features of FastMaps are retained in the data file When stored without the spectral data
12. XRF SYSTEMS IXRF Systems Inc 3019 Alvin DeVane Blvd Suite 130 Austin TX 78741 512 386 6100 Fax 512 386 6105 Web www IXRFsystems com E mail info IXRFsystems com Iridium Ultra Version 1 4 Software User s Guide 7 February 2012 Japan only The power cable packed in the carton is used exclusively for the included EDS system IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 This page intentionally blank 1 2 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 Table of Contents DMC OCUICHION soiicesasetea sca aceccccantaciail ec eaieiealaeabecacete ie a e e A Na 7 Customer SUP POL asasan aa a E easel aieaes 8 2 1 Gras esro at ncaa Unan ter enres recrerepenre en nett itet trcw tren mts itetanr Weimer nT rRteEety arceenny nr peau mate ee renee reenter eter 8 22 SOMWA DU ales En E E santas cat catnn sues sataerannncmins canoe asaaciaeeatuanneeeaiaiass 8 Applicaton OVERVIEW sescsscaisdsscccvccsscaccadescacscesevassudevacceucsoatesudesuadsvassuaseudeccadeuecaeastucesecssnceseudoaceusadsuaneseiees 9 3 1 Te BDA geen erent nmemnnon erertets Smrtico ee es Mma nye ee eer etry een es Macatee a tr Sree nn Teun Arter 10 a2 DD OTS Ali aeee a a ae occa a necuiebyuccussat cosa tneonu cu icdeorse cence 1 3 3 IN TRUS AE EEN EE EA AEAT EE EIEN EE E REEE E E EAT becasue SEET E E E ET A PEE ET TEE 13 3 4 FS VMS t1 EEEN AT E EEE EE EE EA IE EE NEN EPEN TA E EEEE EEE E EE EAE EE E T 13 PAE EN O a a nadin
13. and then aN clicking on the Del Component button Enter the load standard concentrations in the column labeled Conc gor cick hata Print As you enter the assay values they will also appear in the Element table at the bottom of the dialog When you have completed entry of the assay values Hall Quantitation click on the Save button to save the standard file UnAnalyzed Fraction OUO ZVA e Setup an Analysis Settings file with the Quantitative method set to Match This is done by setting the quantitative method for all elements to be Match select Match as the quantitative method on the Quantitation tab of the Spectrum 69 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 Properties dialog as shown below m E e Fillin the Match Setup as described in the description of Qualitative Match Analysis e Save the Analysis Settings so that they can be used on future spectra acquired e Quantitative analysis of a spectrum using these settings will now perform quantitative Match analysis 4 14 3 Viewing Match Results After performing analysis with Match two additional menu items are available for viewing the best matching spectrum and for viewing a graph of the 10 best matching spectra View Match displays a graph showing the 10 best matching spectra as shown below 70 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 Match Spectra q x Print Copy opectrum Fit 3
14. as TIFF or JPEG The software supports export to over 40 file formats This setup allows the user to select only the formats that they use thus reducing the complexity of selecting a file format for export The list below is an example from an Export panel in the software Listed are JPEG TIF 24 and Windows BMP 24 formats All of the other formats are still available and can be added to the list with the Setup Export File Formats menu item Save as type JFE G ASCII JPEG TIF 24 z Windows BMP 24 Selecting Setup Export File Formats displays a panel similar to the following Select the formats that you want to use from the list on the left Click Select All to select all of the file formats click Remove All to de select all lccnit 63 1D tif of the file formats ECCT G3 2D tif cc G4 tif MJEPS eps GEM Image 1 img UIFIF 4 1 1 iff MP IFIF 4 2 2 iff ITIF 4 1 1 jtf EIF 4 2 2 jth EIF 4 4 4 jpg E LEAD cmp LEAD 1 bit cmp MacPaint 1 mac E Microsoft Paint 1 msp 05 2 BMP 1 bmp 08 2 BMP 4 bmp 05 2 BMP 8 bmp 3 4 8 Close 0s 2 BMP 24 bmp Closes the active window P Macintosh PICTURE 1 pct 3 4 9 Close All Closes all windows This menu item has the same function as the toolbar button ut Curent Folder E microdat H Acti Select the windows that you wish to close from the ra ETT aad ar a list The Action column shows the close a
15. behavior and view of the panels by right clicking on Interactive Help Folders the title bar and using the submenu Floating What do you Docking want to do Tabbed Document Auto Hide Work with Hide WI Spectra FOEN Work with ry Digital wie Maves Work with LS eveweies y v ork with ma X ray a ae L Linescans ir Info in Help amp Support Center 19 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 3 5 2 Folders Panel The Folders panel is also displayed on the left side of the EDS application workspace as shown This panel is used to navigate the file system and to open spectra image X ray map and linescan files The panel can be displayed or hidden from the menu item View Folders Operation of this panel is identical to that of the Windows Explorer Clicking on the next to a drive or folder will expand the display showing the files and folders within clicking on the will collapse the display Only EDS data files spectra images x ray maps and linescans are displayed in this panel To open any of these files double click on the file 20 than gt File View Tools Help O ca bed 5 S P Se Acquire Preset 60 0 Folders 1 x ist Desktop A yt My Computer B s C_on_Dell_Insp C lt Ill H O Bac0f32695e4fGead4 O b56423f5bd2762a074 boot Brother H c088253448e47af7b7 CH DELL H Documents and Settin 5 dri
16. calibration point eee 0 000 keV Click again on the Add button this time entering the measured and expected energies of the second peak in our example this would be the oxygen peak measured at 0 650 keV and expected at 0 677 keV Again click on the OK button to enter this as a calibration point Add Energy to Calibration Next click on the Fit button The following dialog will Low Energy Calibration Fit Parameters Appear Force Fit Through Zero The normal settings for this dialog are shown Itis best to eue e ciara start with these values for the calibration Itis important to Plateau Start Energy 0 75 keV make sure that Force Fit Through Zero is not selected To Number of Plateau Points 5 set the displayed values select the OK button 141 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 You will notice that a curve is displayed on the left side of the Low Energy Calibration tab as shown below This curve displays on the horizontal axis the energies that you entered as the measured energies and the vertical axis as the expected energies You can click on the curve and a readout below the curve will display the energy in measured and the resultant energy out expected This can be used to verify that the calibration will work well for the peaks that you have entered 02 03 O4 O05 In Finally select the Enable Calib option You can now acquire a spectrum with this new calibration The l
17. familiar with Windows applications it is recommended that you review the Getting Started book which is provided with your computer system and is also available from the Help menu item on your computer desktop To gain familiarity with EDS analysis the following books are recommended e Scanning Electron Microscopy and X Ray Microanalysis 2 Edition by J I Goldstein D E Newbury P Echlin D C Joy A D Romig Jr C E Lyman C Fiori and E Lifshin Plenum Press New York 1992 e Quantitative Electron Probe Microanalysis gm Edition by V D Scott G Love and S J B Reed Ellis Horwood Ltd Hemel Hempstead UK 1995 e Quantitative X Ray Spectrometry on Edition by R Jenkins R W Gould and D Gedcke Marcel Dekker Inc New York 1995 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 2 Customer Support We are committed to supporting our customers Support can be accessed via telephone fax or 24 hours a day via the internet 2 1 Contacting Us We can be contacted by Telephone 1 512 386 6100 from 9 00AM to 5 00PM Central Standard or Daylight Time FAX 1 512 386 6105 Email support XRFsystems com Internet www IXRFsystems com 2 2 Software Updates We provide free lifetime updates to the original purchaser of the EDS application software via our web site This is a complete installation package for the software To access the latest release of the softwar
18. intensity extraction and quantitation 39 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 4 10 1 Analysis Settings The quantitative analysis steps are set up in the Quantitation tab of the spectrum Properties To access this select Properties from the menu and then click on the Quantitation tab A dialog similar to the following will appear Automatic element identification can be performed prior to quantitation To activate this select the Perform Before Analysis option on the Element ID tab of the spectrum Number of Smooths 1 v Remove Si Escape Peaks Remove Sum Peaks properties Otherwise a manual element ID is necessary Quantitation can be performed automatically at the end of spectrum acquisition To enable this option select Always reed Enea e 0 100 Quantify after Acquire i Ato Setup in spectral processing This performs a Gaussian 1 2 1 smooth of each channel in the spectrum for the specified Deconvolution number of times A value of 2 is recommended for Method Gauss Setup Number of Smooths For noisy spectra larger values can pa be specified For spectra with good statistics this step can Geometry Detector XRF be left out Background Smoothing of the spectrum is recommended as a first step Quantitation It is also recommended that Si Escape peaks be removed To enable this select Remove Si Escape Peaks This method accurately removes
19. is after spectrum processing for example background removal It is sometimes useful to view the data after background removal and it is recommended to view it using bipolar display so that any negative channels can be displayed Below is an example of bipolar display after background removal 21 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 The baseline 0 counts is shown as a horizontal line in the middle of the spectrum display Some channels contain negative counts and thus are shown below the baseline To view the spectrum in bipolar display select View Bipolar from the menu 4 3 Overlaying Spectra Spectra can be overlaid to inspect for similarities or differences This is a useful visual tool Up to three spectra may be overlaid There are three ways to overlay spectra 1 Using the menu select Overlay Spectrum A panel similar to the following will appear 7 x Look in LSDemo ad E o m B 2000 4 My Recent WM 2000 5 Documents WM 2000 6 E WW 2000 7 Woz Desktop Woo W so00 2 S A s000 3 My D t i iy Documents a256 a W s2c0 a er GM 286 b hy Com puter ID do T Files of type Spectrum xsp Cancel Places Open as read only EDS spectrum files xsp and EMSA spectra files can be overlaid Multiple spectra can be selected by pressing the Ctrl key and clicking on a spectrum 2 Using the mouse you can drag a spectrum over ano
20. is slightly different This section of the manual describes the method for doing this combined acquisition and analysis To begin we need to create a new Combined SEM XREF panel This can be done by selecting File New from the menu and then selecting Combined SEM XRF as shown below Create Analysis Data Combined SEM SAF Image Fast Map Fast LineScan Spectrum Report Least Squares Calibration Stages can Stage Map Stitched Images Stitched Maps VP Mode Spectrum Another way to do this is to click on the Combined SEM XRF button res on the toolbar Below is a combined SEM XREF spectrum On the top left is the SEM spectrum and below it is the XRF spectrum To the right of the spectra is the analysis results panel HH cdanew Combined Analysis SEM and XRF Details SEM Anabysis Et Lire tensity Eror Quart Atomic Corc Eror Bree EkgEror MDL icis 2 sig Ys 2 sig Pnt c s 2 sig 3 sig S Ka 000 0000 Ato Of00 O000 wti O000 S347 1462 0000 Fe Ka 1037 0659 Auto Of00 O000 wti 0000 4227 1300 0000 Ni Fa 709 0533 Ato O000 0000 wt O00 3649 1208 0000 Cu Ka 170902 8268 xto 0000 0000 wti On00 36 18 1203 0000 mo Ka 9232 1922 Auto 0000 O000 wte 0000 3426 1 171 0000 Sn La 10420 2042 xto Of00 0000 wti 0000 68 14 1651 0000 2 ch Sb La 000 0000 Ato Of00 OOOO wti 0000 67 19 1639 0000 W a Zn Pb La 1379 0743 amp xto 0000 O000 wti 0000 2200 0938 0000 Ni o pn Cu Zn 0000 0000 wt Total Ni W Cu Pb k 20 0 6 7 8 9 10 Tikeof Ang
21. line to be associated with a peak the line energy must be close to the peak s centroid The Search Width property defines how close the line must be to the peak centroid The value is given in percent of FWHM Full Width at Half Maximum Since FWHM increases with energy lines at higher energies are not required to be as close to the peak centroid as those with lower energies Selecting a larger value for this property will increase the number of element lines that will be associated with a given peak This number should be kept as small as possible Keep in mind that when peaks from different elements overlap the apparent peak centroid may be located a considerable distance from the individual lines Under these conditions a wide value would be necessary in order to correctly identify the elements However this can result in other elements identified that are not actually present Values in the range of 10 35 are typical The default is 12 Always Present Select this to add and delete elements in the Always Present element list Select this and then click on elements in the periodic chart The elements are color coded The color coding is described in the Periodic Table dialog Elements in this list are considered to be in every spectrum collected and will automatically be included in the analysis Never Present Select this to add and delete elements in the Never Present element list Select this and then click on elements in the peri
22. made the x ray map will begin acquisition The element list used for the x ray map is the default element list The default element list can be set from the toolbar properties of any of the EDS buttons spectra x ray maps linescans 9 2 Setting Acquisition Properties The x ray map acquisition properties should be optimized for the specific sample To access the acquisition properties select Properties from the x ray map menu The acquisition properties are found on the Acquisition tab of the x ray map properties panel Properties FastMap1 E Point Dwell is the acquire time per pixel The time is given rT in either milliseconds mSec or microseconds uSec Use microseconds when specifying short dwell times e g below 1 mSec Increasing the Point Dwell time will generally improve the quality of x ray map as larger number of x rays will be accumulated for each point in the image However sample charging effects will be greater with longer times and the total time to acquire a complete frame will increase as well For example a 256 x 256 resolution x ray map with a Point Dwell time of 50 mSec will take approximately one hour to complete a scan If the Point Dwell time is reduced to 1 mSec it will take approximately 1 minute Multi Scan described later in this section is a feature that overcomes these negative consequences of large Point Dwell times Note Point Dwell should always be greater than 3 4 times the value of the Time C
23. nee aaaeadearmieaaaet 86 5 6 Starine the ANY GIS atte cS oe iets sheesh evirstoec deca hice a S 86 5 7 Saving and Loading Location Files 00seneneneeesssssssssssssseeteerresssssssssssseeterrressssssssssssseerrerersssssss 86 6 Working with Spectrum Reports sseseeecocsssssseececcecceccccoccsossecceccoceccoccocossssescccccccccccssssssssssecececeesesssss 87 7 Working with Combined SEM XRE spectra eseceeeoccssssssssscecccccccccccccssssesecccccecocccosssssesescececeeesessss 89 7 1 ACU TID o Pe E Eere a aO 90 42 ident ma SP 9 a tesco huctostsen noc ution esetscet na deeee ycctoen O 90 7 3 OMAN EL TS SC CUE eene E e a a E 90 S Workame With VP SPec aese ooa neo a pA a E o Ea ai 92 8 1 Ea i VP OUNLA OM aeee EEE r a EEN TEER 92 8 2 AGUN NP SPC CW Aisticcsnntistosantecdtaulvaiuatentaddactie setws nid cedtandescaated E 92 8 3 Ouand nS NVP SPCC lid tester sctasanchidaatiuseues aaaledomaatet a 93 9 Working Wath X ray Maps sscicsivctecceseveccecvaceevansccevcdcastucueuaccacucvsessees dscdeueducdeccesssddousseduelsddedesccescees 94 9 1 ACUN Atl Xray M IPn aa sath ussaanarenedashusseeas algalesetanataps aueadceteueataes 94 9 1 1 Preparing the microscope and EDS system for acquisition cccccseesseseeeeeeeeeeeeeeeeeeeeeeeeaas 94 O12 Cheating and Acquiring the X taya E EE T A 94 9 2 DEUS ACQUISITION POPETI S aoreet a cedar aula lcayiah covenants wet laa vou E a wantomtaadlsxsowaniins 95 Jk Remm TOWACGUISINION Locator E E 96 9
24. one hour 1 Select the desired Pulse Processor Filter Time Constant and Full Scale Full Scale does not apply to all hardware configurations If Full Scale does not appear in the panel it does not apply to your hardware configuration The Full Scale can be selected from the Spectrum Properties menu item on the Acquisition tab This is shown at right Normally Full Scale should be set to 40 keV The Time Constant can also as be selected here or alternatively in the Energy Calibration panel as shown below Load Settings 138 WwW a oa 10 11 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 Automatic Manual Advanced FWHM Low Energy Calibration Set Slow Threshold to 0 Start acquiring a spectrum Adjust the Fine Gain until the peaks are within 100 eV of their correct locations While observing the low end of the spectrum adjust the Threshold down until a noise peak starts to appear at the lowest energy Adjust the Threshold higher until the peak just disappears Adjust the Slow Threshold higher until the cut off is slightly below the lowest desired peak Stop acquiring the spectrum a The correct Gain Threshold and Slow Threshold settings for each Time Constant are typically very similar To aide in initial setup of the DPP an option to Copy Calibration Settings can be used If this is the first Time Constant being calibrated it is recommended to use the Copy Calibrati
25. overlay on the spectrum To add notes to a spectrum select View Notes from the menu A Notes panel will appear on the spectrum To edit the notes double click in the Notes panel Below is an example of the Notes panel and its edit panel 29 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 Sample 5776 Date 3 3 2011 Sample of defect area on bearing a 10 Text typed in this window is added as notes for the spectrum and are displayed in the window on the left When you are finished editing the notes click the Close button The Notes window on the left will remain on the spectrum You can move and size this window using the standard Windows mouse interface The display of the notes can be toggled on off by selecting View Notes menu item You can re edit the notes by double clicking the notes window Note When entering text after each line of text press Enter on the keyboard This is especially important for the last line of text 30 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 4 5 Customizing Display and Printing Colors The colors used to display and print spectra can be customized to your personal preferences Some color combinations work well on black and white printers but are not suitable for color printers Users may have color combinations that are preferred for displayed spectra and MLK markers These colors can be adjusted and the preferences saved as default settings
26. peak extraction deconvolution and quantitation e g ZAF Match The steps in the analysis of the spectrum can be customized for particular kinds of samples and stored in Settings Files These settings files can easily be loaded when needed to provide the specific analysis necessary on each kind of sample Automatic element identification can be performed as part of the quantitative analysis see previous section eliminating the need to manually identify peaks in the spectrum prior to quantitation Complete quantitative analysis can be performed by e Clicking on the ToolBar button f e Selecting Analyze from the menu e Setting the Always Quantitate after Acquire option on the Quantitation tab of the spectrum Properties When acquisition of the spectrum has completed the quantitative analysis will be performed automatically The following flow chart shows all the possible steps in order for a complete spectrum analysis Manual step wise quantitative analysis can be performed using the Utility menu item Manual Processing This is described later in this chapter Quantitative Analysis Steps Automatic or Manual Element Identification Spectrum Smoothing Remove Si Escape Peaks Remove Sum Peaks Remove Background Intensity Extraction Deconvolute Spectrum Quantitate e g ZAF Match Some of these steps are optional smoothing escape and sum peak removal and others are mandatory Auto or Manual Element ID background removal
27. rays will be accumulated for each point However sample charging effects will be greater with longer times and the total time to acquire a complete frame will increase as well For example a 256 resolution x ray linescan with a Point Dwell time of 2000 mSec 2 seconds will take approximately 8 1 2 minutes to acquire If the Point Dwell time is reduced to 100 mSec 1 10 second it will take approximately 26 seconds Multi Scan described later in this section is a feature that overcomes these negative consequences of large Point Dwell times Note Point Dwell should always be greater than 3 4 times the value of the time constant used for x ray linescan For example for a Point Dwell time of 50 uSec the largest time constant that should be used is 12 5 50 4 The reason for this is ensure that the x rays acquired for each point are actually from that beam position A finite amount of time is required to process an x ray through the electronics This time is related to the time constant Larger values of time constant require more time to process each x ray 124 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 Resolution is the number of points on the line from which the x ray data will be acquired Larger values for Resolution will require more time for acquisition but will also yield greater spatial resolution in the linescan For example a 512 resolution square x ray linescan with a Point Dwell time of 100 mSec will
28. tab of the Spectrum Properties A dialog similar to the following will appear 2246 2370 ZAF 5 333 5497 ZAF 5 814 5 983 ZAF 6317 6491 ZAF 7385 7ATL ZAF 61 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 Strictly speaking it is not necessary to perform the ZAF analysis only the net peak intensities are required To disable the ZAF analysis you may change the Quantitation Method on the Quantitation tab of the Spectrum properties to None Once the analysis settings have been checked do a quantitative analysis on the spectrum Quantitative analysis can be performed by e Clicking on the ToolBar button rail e Selecting Analyze from the menu e Setting the Always Quantitate after Acquire option on the Quantitation tab of the spectrum Properties When acquisition of the spectrum has completed the quantitative analysis will be performed automatically You may wish to save the Analysis Settings at this time so that you can duplicate the quantitative analysis on future samples This will ensure that the analysis of future samples will be consistent with this analysis of the standard Select Save Settings from Spectrum Properties Create Standard File After performing the standardless analysis select Utility Create Standard from the menu A dialog similar to the following will appear Component Conc Units The Component concentrations are those from the 5 1 514 wt standardless analysis Ensure t
29. take approximately 50 seconds to acquire If the resolution is reduce to 128 it will take approximately 13 seconds The selection of Resolution should be made large enough such that the features that are being observed can be seen clearly and their positions accurately defined Values larger than this add no additional information to the x ray linescan Multi Scan acquires multiple scans of the line of the x ray linescan The scans are summed together producing ever increasing quality in the x ray linescan as the scans are acquired Max Scans is the maximum number of scans that will be acquired The acquisition can be stopped at any time allowing the user to determine when the x ray linescan are of sufficient quality For example a Point Dwell of 100 mSec and Resolution of 256 will complete a frame in about 26 seconds If Multi Scan is enabled and Max Scans is set to 500 the completed x ray linescan will acquire a total of 50 seconds of data for each point This is calculated as 100 mSec x 500 50 seconds The advantages of performing the x ray linescan with Multi Scan are QO The x ray linescan can be stopped at any time from 26 seconds to 3 1 2 hours the time to complete all SOO scans The user can select when the x ray linescan has sufficient quality Sample charging effects are minimized due to the rapid movement of the beam over the line being acquired 10 2 1 Returning to Acquisition Location The microscope stage location is stored at
30. the data file is much smaller but only the maps and the total spectrum can be viewed 9 1 Acquiring An X ray Map 9 1 1 Preparing the microscope and EDS system for acquisition e Select an area on the sample for which you wish to acquire an x ray map e Optimize the microscope for acquiring the x ray map To do this acquire a spectrum over the area to be mapped As the spectrum is being acquired adjust the microscope to get the highest count rate reasonable for the sample This is important because the beam will be moved rapidly from pixel to pixel during the x ray map acquisition High countrates will improve the quality of the x ray maps If the deadtime increases above 40 select a shorter Time Constant X ray maps are typically acquired with a shorter time constant than that of spectra 9 1 2 Creating and Acquiring the X ray map To start acquiring an x ray map click on the Fe button on the Toolbar For integrated EDS systems select an area on the image for the x ray map This is done using the mouse Click the left mouse down to select a corner of the area and then drag the mouse to the opposite corner of the area As the mouse is dragged over the area a rectangle will be displayed showing the area that will be mapped Release the left mouse when finished with the selection To cancel the selection click the right mouse button 94 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 Once the selection has been
31. the following will appear This annotation tool is identical to image annotations and is described in the Digital Imaging manual Edit 134 pix Y 123 pi Fa o O lO a Save Settings As Default tooo w Ekv E Magnification E Micron Bar The annotations are placed only on the map selected To add annotations to a different map close the annotations panel and move the cursor over another map right click and select Edit Annotations from the menu again 9 17 3D Viewer To view a map as a 3D surface select View 3D from the menu After selecting View 3D a panel similar to the following will appear Select the element to view in the list on the left side Click on OK to create the 3D view of the map The intensity of each pixel in the map is used as a height Z axis thus forming a surface from the data Below is an example of the 3D view 115 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 oom MNO Sey Gx Mv srz Move ARotation D Move Rotate Render Fast Auto Render Fast Full Render 512 Mg 3D 08 Color r4 Zoom The 3D viewer has a control panel on the left side for manipulating the view and the image view on the right side There are three control panels 3D Color and Zoom Clicking on the respective tab at the bottom of the control panel selects the specific panel 116 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 9 17 1 3D Control Pa
32. the peak positions there is a well characterized equation that relates peak position energy to the spectrometer zero offset and gain eV channel Both these are allowed to vary independently but the calculated must be within both the values defined in the deconvolution setup default zero 40 eV and default gain 0 2 This technique is much slower than the linear method especially when analyzing many elements but it may be necessary for some samples 52 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 To select the kind of Gaussian deconvolution click on the Setup button in the Deconvolution area on the Quantitation tab of the Spectrum Properties as shown to the right A dialog similar to the following will appear Selection of Restrict to Linear Peak Fit determines which kind of Gaussian deconvolution is to be used Selecting Diagnostic Output will display the fit spectrum overlaid on spectrum This can be useful in evaluating the quality of the deconvolution When using the linear peak fitting you can visually examine the fit to determine if the FWHM requires adjustment if the fitted peaks are wider or narrower than the spectrum peaks and also the energy calibration where the fitted peak positions line up with the spectrum peaks The system FWHM can be adjusted in the SS l Acquisition tab of the spectrum properties A value for FWHM is stored for each pulse processor time constant in the sy
33. the selection of the font and font size Eepe used athe report Pleasenote that the MV Spectrum M Quantitative Analysis D Image Spectrum Options report title will be 2 points larger than the Heading File Select Disable Report Options Text Font Size Image Height Sets the height of the image in inches Spectrum Height Sets the height of the spectrum in inches Fit to 1 page When selected this option will format the report to fit on one page within the limits set see below If the initial settings of font image and spectrum height result in a document which is larger than one page the font and heights are reduced so as to fit the report to one page The font and heights will only be reduced in size to the minimum limits given below The heights are reduced in increments of 2 inch The font is reduced by 2 point size for every 1 inch that the heights are reduced Fit Minimum Sizes These are the minimum values allowed in the document when the Fit to 1 page option is selected e Text Font Size Sets the smallest font that will be allowed in the document e Image Height Sets the shortest height that will be allowed for the image in the document e Spectrum Height Sets the shortest height that will be allowed for the spectrum in the document 38 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 4 10 Quantitative Analysis of Spectra Quantitative analysis performs spectrum processing net
34. the start of Properties FastLineScanl acquisition To return the stage to the location of the Acquisition Element Selection Quantitation previously acquired data select View Go To Stage Location H He This will move the stage to the location where the data were cee ae NE 3 Na Mg Al Si P S Ci Ar acquired K c s t V ME o z Ga Ge as Se Br K Rb Sr Zr Nb Mo Te Ru Rh Pd Ag Cd In 3n 5b Te I Fe Cs Ha La Hf Ta W Re Os br Pt Av Hg TI Pb Bi Po At Rn Fr Ra Ac Ce Pr Nd Pa Sm Ev Cd Tb Dy Ho Er Tm b Lo 10 3 Setting Element Properties Th Pa U Np Pu Am Cm Bk Cf Es Fm The element list used for the x ray linescan is the current element list from the last EDS acquisition For example if a spectrum was acquired and peaks were labeled either Remove Al VIDA manually or using automatic peak identification the labeled f Scale al ee 0 Maximum Minimum Maximum elements will be the element list for the next x ray linescan acquired Element Settings ROI Width 1 8 FWHM Restore Defaut ROI Further refinement of this list can be done with the Element Selection tab of the X ray LineScan properties To access the x ray linescan properties select Properties from the x ray linescan menu Ty High keV Shown is the Element Selection tab The elements that will t E 5 292 5 537 be acquired are indicated on the periodic chart i
35. will appear next to this menu item Selecting this again will stop acquisition Clear erases the spectrum Resume continues a previously stopped acquisition or starts a new acquisition if no spectrum has been acquired This can be useful if you wish to acquire for a longer time that originally set 4 1 1 Returning to Acquisition Location The microscope stage location is stored at the start of acquisition To return the stage to the location of the previously acquired data select View Go To Stage Location This will move the stage to the location where the data were acquired 4 2 Viewing Tools 4 2 1 Expanding and Contracting views The most common way to adjust the view of the spectrum is using the Cursor To adjust the view of the spectrum press the left mouse button down at a location on the spectrum that you would like to view at the center of the window With the mouse button held down dragging the mouse will have the following effects e Drag Right will expand the spectrum horizontally displaying more detail in the spectrum around the Cursor location 6 fd fA fit e Drag Left will compress the spectrum horizontally displaying a larger range of energy in the spectrum window 26 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 e Drag Up will expand the spectrum vertically displaying more detail in the spectrum e Drag Down will compress the spectrum vertically 4 2 2 Auto Vertical Scale Auto V
36. 0 724 2 441 0 918 0 821 5 433 661 2 004 0 000 0 178 0 019 0 011 0 669 0 656 94 453 1 888 0 002 0 004 0 116 662 1 919 0 041 0 340 0 081 0 038 0 286 1 036 95 461 0 556 0 082 0 159 0 000 663 2 093 0 168 0 666 0 047 0 302 1272 1 491 93 596 0 287 0 033 0 032 0 014 Mean 2 005 21 409 0 395 0 049 0 127 1 576 0 977 74 415 1 027 3 175 2 892 0 066 0 039 0 065 0 044 Std Dev 0 087 42 678 0 249 0 031 0 133 1 717 0 380 40 403 0 154 5 149 3 593 0 000 0 041 0 083 0 064 Min 1 919 0 000 0 178 0 019 0 011 0286 0 656 2 441 0 918 0 287 0 351 0 000 0 002 0 004 0 000 Max 2 093 85 426 0 666 0 081 0 302 4 079 1491 95 461 1 136 12 321 5 433 0 000 0 082 0 159 0 116 The following menu items are available for Spectrum Reports File Export Stores the Spectrum Report in an external ASCII text file The format of the file is a tab separated column text file which is compatible with Microsoft Excel spreadsheet It can also be imported into word processors such as Microsoft Word File Print Prints the Spectrum Report Note that the report is printed on a single sheet of paper The font is adjusted so that the table will fit on the page in the current page orientation Landscape orientation is often desired for printing of reports Edit Copy Places a copy of the table on the Windows Clipboard This can be pasted into Microsoft Excel spreadsheet or into word processors such as Microsoft Word View Material When material classification has been calculated for the spectra disp
37. 03 8 59 AM 1 6 1996 5 14 AM 1 6 1996 5 14 AM 1 6 1996 5 16 AM 1 6 1996 5 20 AM 1 6 1996 5 19 AM 2 23 2011 2 33 PM 1 6 1996 5 14 AM 4 7 2003 8 59 AM 1 6 1996 5 14 AM A 5 14 AM PLT Fill PLT Fill PLT Fil PLT Fil PLT Fil PLT Fil PLT Fil PLT Fil PLT Fil PLT Fil PLT Fil PLT Fil 7 Restore Default ROI IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 Setup Palette Files Palette Files Assigned to Hements Palette Files Elt Palette File oa Assign To J Edit ait Remove Assignment To assign an element to a palette 1 Select the element s in the list on the left side panel by clicking on the gray button to the left of the element name 2 Select a palette from the list on the right side of the panel As you select the palette it will be displayed in the box to the right of the list of palettes 3 Click on the Assign to Elements button This will assign the elements selected in step 1 to the palette file selected in step 2 To remove an assignment of an element to a palette 4 Select the element s in the list on the left side panel by clicking on the gray button to the left of the element name 5 Click on the Remove Assignment button You can also edit the palettes in this panel To edit a palette 1 Select a palette from the list on the right side of the panel 2 Click on the Edit Palette button A panel similar to the following will appear This p
38. 15 1 1 Editing the Calibration The attributes of the curve fit are mostly set with the editing panel shown below Least Squares Calibration File PEEEEEEE E E x E E E E x E microdat L3Demo 661 xsp EAmicrodat LSDemo 662 xsp E microdat L3Demo 663 xp The table at the top of the panel displays the list of elements in the calibration file Elements can be removed from the calibration by selecting them in the table and clicking on Delete Element Elements can be added to the calibration by clicking Add Element Only elements that are specified in the standard file can be added The table at the bottom of the panel displays the standards A standard can be removed from the calibration by selecting it in the table and clicking Remove Standard Standards can be added to the calibration by clicking on Add Standard Each element has a Type Type allows you to specify if the fit will be forced to include 0 or not Selecting linear type will not force the fit through 0 selecting linearO will Below is the carbon calibration with both linear and linear0 types linear linearO 75 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 Each element has an Order Order defines the linear order of the curve fit Order 2 fit is a straight line Order 3 fit is a parabolic fit An order 2 will fit any two points to a straight line If there are more than 2 points standards then a straight line may not exac
39. 21 X5P 0 180 Spectrum xSP 0 225 spectrum 5P 0 226 Imagel 2 25P D227 test 4SP 0 228 Imagel 4 x 5P 0 229 Imagel 3 45P 0 230 Imagel 1 45P 0 231 View Match Spectrum displays the best matching spectrum a shown below Best Matching Spectrum 371 Jee oe AUUE Cursor ert 52357 Window 0 005 40 955 26rSr0 cnt 4 15 Least Squares quantitation method Least Squares LS quantitation method uses a set of EDS standards to define the relationship between element intensities and concentrations Similar to ZAF with standards LS requires that the user acquire a set of EDS standard spectra and to also create EDS Standard files The LS calibration is then used to calculate a best fit curve using the intensities from the standard spectra and the concentrations from the standards files This technique can be useful with samples that have very low concentrations or when ZAF quantitation does not perform adequately 1 e carbon 4 15 1 Creating the calibration file Select File New from the menu and then select Least Squares Calibration as shown below 71 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 Spectrum Combined SEM AF Image Fast Map Fast LineScan Spectrum Report Least Squares Calibration Stages can Stage Map Stitched Images Stitched Maps VP Mode Spectrum ma Ja standard Update Graphs We must first add some standards to the calibration Click on Add Standard to do th
40. 3 Delta Element Proper ieS ls esjnasenieacavactoncsvedonla cauiaibsueaxts seen ET 96 Adjustins Color Palettes Tor X ray Maps arnee na AT N E A te vechhicedenis wuierbedenncsowstioln 98 Oo SUP PEET ESEE E 100 9 4 CCl ANNA E a e A casita 101 9 5 Mew HOS Ie E a uugtailocat canta lacs 102 9 6 The Sum Spectrum and Maximum PIKE luer a E a N 103 HOF Element S EC UON aa a N EE saline etaveeacuensveiaans 104 9 7 EXPONE XA TV MIPS a E aia cel obsess neauahecieemene Wades 104 9 8 Viewing Intensity Composition of Points on X ray Maps ccccssesesssseseeeeceececeeeeeeeeeeaeaeeeeeees 105 gsl Mode anea a n e ae teas a E hensdee se ceoeaaeeass 106 9 52 Locanons Momeni a a N E N E E O E ET 107 9 9 Overlaying X ray Maps Composites essssssssssssssseeeerressssssssssssssssseetereerossssssssssseeerereessssss 108 910 Element Quan tative X ray Maps sccccxcccsecssseisdiccossaseceuceiodueaseidetetcas Eea lee E EE NES 109 9 11 Component Quantitative X ray Maps ccccccccccccccccceeeessseeseeeececeeeeeeeeeeaaaeseseseeeeeeeeeeseeeeaaaas 110 O42 Niewine Omini ve Maps e e a 110 9 13 Quantifying X ray Maps Composition soxcsvivevcesisaciclenavautesavoase conve Qedeedecuiteedienntourenaewersdataaeess 111 gA Seater PlOU AMAL y S S a a eae suabamecatane 113 913 Extracto Linescans FOTM aDS seie a i eaae 114 ONG ADIOS MIPS nae owe ate tet once amiu naeoti ea meee neetineeaneeameunanmaeerueaen 114 DAT SDD NAE WEP vasaussisaceaioawasahdeiraig
41. 833 att Total complete analysis for both spectra Below is an example kV 20 0 Takeodt Argzle 350 Bec Ore Simm Peak Cit smooth l Ekg Abo Elapsed Liretome 100 0 Preset 100 Iode Tome ass Fit TEST in HEF Analysis Et Lie htersiy Emor hwet Con Emor ici J cizZ J cizZ 5 Bia O00 O000 Ato 000A whe 6O000 Fe Ka S950 1543 Awto 0093 wh O018 Hi Ea 4256 1305 LAF 0351 wii O08 au Ha scot a 18551 LAF 51583 whi 0173 m Ea 64956 S097 Wto 8426 whe 0050 Sr Ea 4967 1410 Auto 5858 wht 0 166 5b Ea O60 0 155 Wto O 125 whe 0033 Po La S109 1801 sto 65 164 we O 115 LOO 000 we Total kV 350 Takeo Argzle 45 0 Esc Or Simm Peak Cit Sm otk l Ekg Abo Elapsed Liretme 100 0 Gees Fit S4T 91 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 8 Working With VP Spectra When acquiring spectra in variable pressure mode VP mode quantitation of spectra needs to account for the effects of the gas in the chamber To properly account for these effects one should use the VP Spectrum for quantitation instead of a standard EDS Spectrum 8 1 Enabling VP Quantitation To enable this feature in the software select Tools System Setup from the menu and click on the Options tab Select Enable VP Quantitation After the selection you must restart the software to complete the selection 8 2 Acquiring VP Spectra Spectrum ee Combined SEM AF Select File New from the menu A panel similar to the following Image Fast Map will a
42. 93 1 000 LK 3 FastMap 65 993 22 548 750 LK 4 FastLineScan 65 885 22 446 1 800 The buttons in the center of the panel Spectrum Image FastMap etc are used to select data to be acquired at the current stage position The top portion of the panel deals with how the data will be stored e Sample Name sets the base name for all of the data acquired In the above example LK is the base name e Save Data Selecting Individual Files will store each EDS data Spectrum Image FastMap etc in separate files Selecting EDS Dataset will store all of the EDS data in a single EDS DataSet file In this example there are four data to be acquired labeled LK 1 through LK 4 At the bottom of the panel is a list of the data to be acquired the X Y stage location if the SEM is equipped with a motorized stage that our software can control the magnification to be used and whether or not the operator wishes to execute Auto Focus and or Auto Brightness Contrast if those options can be controlled by the EDS software This varies by microscope vendor and model The Delete button is used to remove one or more entries from the list Select the entry s by clicking on the buttons on the left side of the list hold the shift key down to select multiple entries and then click the Delete button 130 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 The Go To button is used to navigate to a selected entry in the list Selec
43. Next Spectrum will copy all MLK markers from the present spectrum to any subsequent spectra acquired This can be useful when taking several similar spectra on a sample It is not necessary to label the peaks on subsequent spectra Below is an example of MLK markers displayed on a spectrum Properties IXRF Calibration Std 2 4 7 6 Automatic Element Identification Automatic element identification Auto ID is a tool that a automatically locates the peaks in a spectrum and associates the most likely elements with each of these peaks E Setup Automatic peak identification is invoked with the ToolBar Ei 1D List Always Present gt Never Present Clear List Acquisition Bement ID Quantitation Display button ES It can also be added to an analysis as an automatic step performed prior to the quantitation of a H He spectrum see the Element ID tab below Auto ID a Be eee Ne i Na Mg Ai si P s c E examines all the peaks and all the identified lines and K Cs Sc Ti V Cr Ma Fe Co Ni Cu Zn Ge Ge As Se Br Ke attempts to predict the most likely combination of elements Rb Sr Y Zr Nb Mo Te Ru Rh Pd Ag Ca In Sn Sb Te 1 E that qualitatively match the spectrum For any given Te ae SG ORE ea EA Ra element all possible peaks in the spectrum are considered Ce Pr Nd Pm Sm Eu Gd Th Dy Ho Er Tm Yb Lu when making the most likely estimate of elements present Th Pa U Np Pu AmCm Bk Cf
44. Plot Detail Select Area The Scatter Plot Analysis data displayed can be Printed Exported and Copied from the panel s menu 9 15 Extracting Linescans from Maps It is sometimes desirable to extract a linescan from a map This process extracts the spectra data from a line defined by the user on the x ray map The linescan is not acquired from the sample the spectral data is taken directly from the stored x ray map spectra This allows for the viewing of a linescan from an x ray map after x ray map acquisition has taken place To extract a linescan from a map 1 Select the menu item Process Create Linescan from Map A panel similar to the following will appear EEE a y Create Linescan From M l a line on either the microscope image or one of the fay maps The Linescan 2 Move the mouse over the map to the starting location of the desired linescan Press the left mouse button down and drag the mouse to the end location for the linescan Lift the left mouse button 3 A linescan will be generated from the map data 9 16 Annotating Maps Annotations can be added to each map and the SEM image To add annotations position the cursor over a map and right click From the menu select Edit Annotations as shown below 114 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 Fe wth C wto File eee Edit Copy Ctrl C Acquire Annotations View Process Properties A panel similar to
45. T D E T 33 aes SCrOLM AS Peak Tdentifie isien E 33 4 7 4 Cursor Identification eeeeeeeeeesessssssseeeeeereressssssssssssseceteeresssssssssssssectrreeessssssssssssseeereeeesesssss 34 4 7 5 Customizing Display of MLK markers ccccccccccececceeceeeeeseseseeseeecceeeeeeeeeeeeeeeaaaaeeeeeses 34 4160 Automatic Blements Iden Mal om sreeoie a ea ee E 35 4 7 7 Configuring Automatic Identification ccccseesssssseecccceeccccecceaeseeesseeeeeeeceeeeeeeeseasaeeesssesees 35 4 8 Customizing Spectrum Rendering for Printing Exporting and Clipboard ccceeeeeeeeeees 36 4 9 BE OO ITN NG S08 oh ctaacos a e taawiees ned mbes E edeeameese cena 37 LIE BIC EE XDOE SPCC WIN oe ashucecdetnscuicasersensa E e E E N vet 38 AOD FICE POr ADAIN SIS arin A E A 38 2935 Pes xX pot MUS pec im EXPO tsaa a 38 AO FIE EX POME SPO OW Ord aroni 38 ALO Quan AUVAI Sis OL SPEC aese E E betel 39 4 10 1 PRTVAINY SUS oeM OSs a E E EA E E AAN 40 4 10 2 Usmo StorcMometr y OXIdES CIE horrira e oniaesionoaentaveutnadelexlavtiad 42 4 10 3 Minimum Intens iy CAE demeni E TEE A 44 4 10 4 Sample Odin and THICKNESS deei AA 44 4 10 5 Cuast mizin Repo OUMU een E E A achonasdeoxlausiad 45 4 10 6 Using the Manual Processin Toolhiireuu iea ined E TA axle vv 46 4 10 7 Back cround Mode iS vssisesersniavachonnneslantaways aeeelvedion awakes sovewien la uacicneseodextaueehnesded ox tavavaatas 47 4 10 8 Bae k CROW PIC oie ass oli Creep Satta adama
46. ach reading of the Input In the example shown the Sample 200 Period is 1 microsecond There bat 0 1000 2000 3000 4000 S000 6000 TOO0 S000 H Ser microseconds Note that for long Sample Period 1 000 p Sec Sample Periods a significant delay will occur while the data are being collected An hourglass cursor will appear on the screen during this time to indicate that the system is busy with the sampling of the input are 8000 samples taken so the total time displayed is 8000 14 6 Calculating Detector FWHM Accurate quantitation of spectra requires measurement of the FWHM Full Width at Half Maximum of the detector This measurement is used for example in the gaussian peak deconvolution during spectrum quantitation FWHM can also be an indication of the health of the detector Increases in the FWHM can indicate a failure of the detector FWHM is the measure of the width of a peak The Mn Ka peak is used by most manufacturers of detectors for specifying FWHM This is also the peak width used by the quantitative analysis software Peaks at higher energy will typically have larger FWHM values and those of lower energy will have smaller values This is accounted for in the software Only the FWHM of the Mn Ka is required FWHM is measured at each of the processing time constants Larger time constants will produce smaller values for FWHM Smaller values of FWHM are desirable for quantitation as this makes the decon
47. aks in the spectrum If you think of each line series as a fingerprint then these fingerprints can be manually selected and visually matched to the spectrum peaks Of course the lines are broadened by the detector response function so one should align 34 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 the individual lines to the peak centroids making allowance for peak overlaps for adjacent lines For example most Ka and Ka lines are too close to be resolved by EDS detectors so these will appear as one broad Ka peak The lines in any series all have different probabilities so that there is significant variation in the relative heights of each line The MLK markers are displayed on the spectrum at the energies of the lines This visual aid is used to verify the presence of an element in the spectrum Each line can be labeled with its element symbol e g Fe although displaying all of the markers and labels on a spectrum can create a very cluttered view Using this dialog each label and marker can be selected on or off The markers can be scaled to the parent peak This is the default selection When selected the marker for the parent peak of each line series K L M will be displayed at the height of the spectrum data in its channel The markers for the remaining lines in each series will be scaled to the parent marker s height based upon the relative probability of the line in the series Selecting Keep MLK for
48. al Rev 1 4 3 Application Overview a jram Lb am OFHRS te 2 eee iem dhh KALA aT H EOR C E j DA Mig toe iie App empo iga om Ua DEn urs Pt iii ram in a ice L 4 H maha i w a oe Ie Ee m el eee mei ii hee Milo De Fa kal Ba et fa ka Emiri Wii A e pd oe lt All acquisition and analysis tools provided by the EDS software are contained in a single application Shown above is an example of the four major tools provided by the software e Digital Images e EDS or XRF spectra e X Ray linescans e X Ray maps Each one of these tools is loaded as necessary IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 3 1 TitleBar TitleBar Menu Bar ak Iridium Ultra Ceramic File View Edit Setup Acquire Process Properties Tools Window Help DEALS au Ge aT A S Tiel ESR H Acquire Preset 10 0 Livetime Livetime 10 0 0gs 121 0 kV 20 0 Mag 100 Z ToolBar At the top of the application is a TitleBar Displayed in the TitleBar are the name of the application and the name of the active window Spectrum1 in this case As you work with the software you activate a window by clicking on it with the left mouse button Activating a window will do the following e Place the name of the active window in the TitleBar e Update the menu Each type of window spectrum image etc has its own unique menu designed specif
49. alette Green 9 i and this is the palette created by these ranges In this color palette only the color Red is used For the least intense values in the map the brightest red value 255 is used Likewise for the most intense value in the map the least bright value 0 is used Blue OU 0 i 9 3 1 4 Color Palette Files Default color palettes are used when creating new x ray maps The Color Palette default color palettes are stored in files in the directory that the EDS application is installed The files are named defpal1 plt defpal2 plt defpal8 plt These files are provided with the application but can be replaced with color palettes created by the user Pseudo Gray Two functions in this dialog allow for viewing and saving these ae color palette files These are the Load File and Thermal Save File functions Load File To view a color palette file click on the Load File button A Save Fie dialog similar to this will appear Spectrum Window Color Change 99 IXRF Systefj Look in di Palettes Select a file from the list and click Open The color Sy palette will be displayed in the dialog as shown below This is the file defpal1 plt Recent Places Note the color palette files are stored in the folder c ixrf palettes _ DEFPAL PLT _ DEFPAL8 PLT _ defpala plt _ defpall0 plt _ defpall1 plt File name Files of type Image
50. and ensuring that the peaks are at the correct energies For example you may wish to use the aluminum and copper calibration material that you probably use for energy calibration In the Low Energy Calibration tab ensure that the Enable Calib checkbox is not enabled as shown here m Enable For the calibration it is necessary to ensure that the Low Energy Calibration is not enabled Calib You will now need to acquire a spectrum that has light element peaks in it You will need two peaks for the calibration Carbon and Fluorine are good choices Oxygen can be used in place of Fluorine if Fluorine is not available You can use two spectra the peaks don t have to come from a single sample What you will need is the measured peak energy of the peaks For example if you have a spectrum containing carbon and the measured peak energy is 0 252 keV we know that it is expected to be at 0 282 keV weighted average Ka peak of carbon Likewise if you have a spectrum maybe the same as the first spectrum with oxygen in it and the measured peak energy is 0 510 keV we know that it is expected at 0 523 keV Once you have these values of measured peak energy and expected peak energy click on the Add button The following dialog will appear Enter the energy that you measured the peak to be at in our example this is 0 252 keV and the expected energy in our example 0 282 Note that these energies are given in keV not eV Click on OK to enter these o as a
51. anel is described above in section 7 4 9 4 Spectral Imaging 101 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 Spectral Imaging provides a multi element overlay over the SEM image in a FastMap Above is an example of a typical Fastmap with spectral imaging Notice that the panel that normally displays the SEM image is colorized and has overlays corresponding to the iron and carbon maps Some of the key features of spectral imaging are 1 Overlays dynamically update during FastMap acquisition 2 Element overlays can be added removed dynamically during acquisition 3 The element overlays utilize the threshold settings to improve the overlay display There are two basic display modes for FastMaps 1 Individual Maps Mode This is the typical display mode where all elements are displayed in individual panels in the FastMap window 2 Overlaid Maps Mode No individual maps are displayed Only the SEM image is displayed Elements can be overlaid on the SEM image Selection of the display mode is done with the menu items View Individual Maps Mode and View Overlay Maps Mode The last selected display mode is retained for subsequent new FastMaps The display mode is also retained in each FastMap file so each map will be displayed as they appeared when they were saved The Element Selection property panel refer to section 9 3 page 96 allows for selection of display mode and threshold for each element and overlay s
52. antitative analysis the spectrum being analyzed is compared with spectra stored on disk that also have accompanying standard files which define the composition of the standard spectra As with the qualitative analysis the best matching spectra are displayed After this display the best matching spectrum is used with its standard file to perform quantitative analysis of the spectrum Both spectra are processed Escape Peaks Background Removal Deconvolution and the quantitative analysis of the spectrum is based upon a simple ratio formula given below 66 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 ConcSpectrum ConcBestMatch IntensitySpectrum IntensityBestMatch Where ConcBestMatch is the concentration for an element in the best matching spectrum s standard file IntensitySpectrum is the element net peak intensity from the spectrum IntensityBestMatch is the element net peak intensity from the best matching standard spectrum ConcSpectrum is the calculated element concentration in the spectrum The spectrum comparison process is as given below The spectrum being processed will be referred to as the sample spectrum 1 A standard spectrum is loaded from disk This will be referred to as the match spectrum 2 The match spectrum is normalized to the sample spectrum using the Normalization Region defined in the Match Setup The match spectrum and the sample spectrum are integrated over the Normalization Region
53. are acquired Thus spectrum x ray maps and x ray linescans look somewhat realistic for demonstration purposes The default spectrum is a steel spectrum Clicking on Use This Simulation will store the current spectrum as the synthetic spectrum Clicking on Reset to Default will restore the synthetic spectrum to the steel spectrum 84 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 5 Working with Automatic Multiple Spectrum Acquisition Using the Multi Spectrum tool it is possible to automate the acquisition and analysis of many spectra on a sample This is useful when a sample has several distinct locations that need to be analyzed To access the a Multi Spectrum panel select Setup Analysis Positions from the image menu or select the alia button from the integration toolbar Below is the Multi Spectrum panel that will display after your selection Acquisition and Analysis Settings jac jut Clearust Delete Points Save Anais Postion Fie ore eee Add Labeled Load Analysis Positions File Name x Y Use Present Settings E Acquire Save Spectra In Directory CIMRFDATA Browse Generate Spectrum Report Print Options Reports Auto ID Spectra 10 keV 5 Cursor Vert 5 Window 0 005 40 955 O0 cnt 5 1 Selecting Locations Select Spot Mode Ee Raster Area akaa and select one or more locati
54. ariations in elemental composition An x ray linescan is performed by acquiring x ray data at evenly spaced points along a horizontal line on the sample The x rays are displayed on the screen as line graphs one for each element in the element list for the linescan As an example the x ray linescan below displays the distribution of Si Pd Fe and Cr LineScan oy Ea Our EDS software provides an advanced type of x ray linescan which we call FastLineScan FastLineScans acquire and display the x ray linescans for all elements in the element list and also store information that allow for viewing the full spectrum from each point on the linescan Below are the advanced features of the FastLineScan Ability to view total spectrum from the x ray linescan Ability to view the spectrum from each point on the linescan Display a linescan for any additional elements desired without re acquiring the x ray linescan FastLineScans can be saved with or without the spectral data When stored with the spectral data all of the features of FastLineScans are retained in the data file When stored without the spectral data the data file is much smaller but only the linescans and the total spectrum can be viewed 10 1 Acquiring X ray Linescan 10 1 1 Preparing the microscope and EDS system for acquisition e Select an area on the sample that you wish to acquire an x ray linescan e Optimize the microscope for acquiring the x ray linescan To do thi
55. button 4 16 3 Select or Create a Materials Class fe ew soa A Material Class or Material Classification is as described at the beginning of this chapter It contains one or more material composition specifications To select or create a Material Class click on the Select button A dialog similar to this will appear feled Maten Cia The Materials Classes that exist in the database will be oo OK il displayed If none exist or you wish to create a new Materials Class click on the New button A dialog similar to the following will appear Enter a name for the new Materials Class and click OK After creating a new Material Class it can be selected in the Select Material Class dialog above After selecting a Materials Classification it may be necessary to edit it to add or modify the materials specified Click on the Edit button A dialog similar to the following will appear IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 The table displays the material names in the left most column and the elemental composition in the columns to the right The ranges of elemental concentrations for the materials can be entered minimum and maximum values for each element and elements can be added or removed from the specification Element concentrations are entered as a range minimum and maximum To specify that a given element is not significant in a material enter the values of 0 for minimum and 100 f
56. cally unique To select a pattern click on Select Pattern On Image Then select a rectangular area on the map area around the pattern you wish to use You can test the pattern after selecting it by pressing the Test Selected Pattern button The result of the test should be within pixel If the test yields results greater than 1 pixel you may want to consider selecting another pattern on the image or adjusting the image acquisition parameters for better image quality Drift correction is performed at the end of a map frame It can be performed at a specified time interval or number of frames For example if you want the correction to be performed every 30 seconds select Every in the Check Drift area and input 0 5 in the Minutes edit box Or if you want the correction performed every 5 frames select On in the Check Drift area and input 5 in the Frames edit box The drift correction will be performed repeatedly based upon your selection of the interval time or frames It is possible that insufficient border area was reserved for drift correction In this case you can select whether to stop the map immediately or to let the map continue Use the option Stop if sample drifts out of range 122 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 10 Working with X ray Linescans X ray linescans are excellent tools for determining the location of phases particles and other features on a sample that can be discriminated by v
57. ction B FastMap FastMap Save Automatic that will be done for each window By default any PP FastLineScan Fast Linescan Save Automatic window that has been acquired and not saved will E vee Image Save Automatic i Combined SEM XRF1 Combined SEM XRF Spectrum Save Automatic be saved automatically before closing The data will be saved in the Current Folder Note in the example that Spectrum action is No Action Required This is because Spectrum has already been saved and does not require saving before closing The other data shown FastMap1 FastLinescanl etc have not been saved and the default action Save Automatic will be applied 16 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 The actions are e Save Automatic Saves the data in the Current Folder using the Name given e Save As Displays a Save dialog for the data allowing you to select a different name and folder for the data e Don t Save This will close the data without saving it The previously acquired data will be lost e No Action Required This is the default setting for data that has already been saved It is equivalent to Don t Save 3 4 10 Save Saves the contents of the active window using the name in the application TitleBar 3 4 11 Save As Saves the contents of the active window allowing you to change the name of the file 3 4 12 Export Saves the active window in an image format Many graphic image file formats are a
58. d channel energies e g between 5 953 keV Selecting Use Background Removal will automatically calculate a i background under the peak and remove it prior to calculating the FWHM The caleulaicd a eround 1S displayed as shown Print Prints the FWHM calculations Copy Copies the FWHM calculations to the Windows clipboard 144
59. d manually by entering a number here Number of Fields Vertical This is the number of images vertically in the stitched image This is calculated automatically when you select an upper left and lower right corner The automatic calculation can be changed manually by entering a number here 133 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 X Overlap and Y Overlap There can be an error in the stage positioning for each of the images To allow for this error an overlap can be specified as a percent of the width and height of the image Typical values of overlap are 1 5 Acquire in Serpentine order Normally images are acquired left to right on each row of the stitched image map With this option selected the images will be collected left to right for the first row right to left for the second row etc This will improve throughput but may lead to some additional misalignment of the images due to backlash in the stage Resolution This is the pixel resolution of the image s maps s being acquired The software supports 4096 x 4096 pixel resolution images and maps Care should be taken to ensure that this maximum resolution is not exceeded when setting up the area to be acquired Present Location This displays the present location of the stage The stage can be moved via the software by clicking on the Move To button OK Clicking on OK will start the acquisition 12 2 Editing Below is a 2x2 stitched
60. d of quantitation Spot Size sets the pixel size for the processing It is best to examine spectra from points on the map using View Intensities and Concentrations to get a good idea as to the total counts in the spectra of the map Increasing the spot size will combine adjacent points spectra to create a spectrum with more total counts and usually better formed peaks This can be important when performing background and overlap corrections When Display Processing is selected the individual pixel spectra are displayed during quantitation This could be useful for setting up the quantitation and diagnosing quantitation issues but it slows down the process of creating the map by 20 De selecting this option will create the maps in a shorter time period 109 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 Start Click on Start to begin the quantitation of the maps The button will change to Stop Pressing this button will cancel the quantitation process 9 11 Component Quantitative X ray Maps Individual component x ray maps calculated from quantitative analysis on the maps can be generated Acquire Clear File Edit View Process Create Quantitative Element Maps Create Quantitative Component Maps Properties This feature will produce maps of the components e g oxides that have been set up in the x ray map quantitation properties Select Process Create Quantitative Component Maps from the me
61. d together A spectrum is created it is analyzed and the intensities or concentrations are displayed in the histogram The freehand location is labeled and displayed on all of the maps and the image The labeled data are added to the Locations list on the histogram If Show Spectrum is selected the spectrum is created from the area and displayed 9 8 1 7 Locations List When one or more Rectangle Freehand or Saved Spots have been created on the x ray map the Locations list is visible on the right side of the panel If the list is not visible grab the border of the panel and drag to the right to show the list of locations The Locations list displays the Rectangle Freehand 106 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 and Saved Spots Below is an example of the locations list with three locations Selecting a location from the list will re display the histogram data for that location Intensities and Concentrations are available for display in the histogram and are also displayed in the Locations list Locations can be deleted from the list by selecting one from the list and clicking on the Delete button SEM Sample 7 Element Intensities Concentrati Locations Intensity Concentration Locations Mode Delete Off Keep Generated Spectrum a Location Fe Gr SOO Spot Spot Size Save Spot _ E 20 497 154 158 Cnts Rectangle 2 15 853 188 858 a 15 472 192 021 Freehand 100 0K
62. e do the following e With your internet browser go to the web site http www IXRFsystems com e Click on the Support button at the top of the home page e Click on the Downloads button on the left side of the Support e Please read carefully the instructions or Release Notes on the Software Downloads page The instructions on this page may change as new releases are provided For example a new driver for the MCA card may be required and this may require additional steps to be taken to complete the installation of the latest software e A password is required for most of our software and user manuals installations To obtain the password contact us by telephone as described in Contacting Us The software update installation is typically a two step procedure 1 Download the software If you have replaced your computer you will need to download and install the Support Files EXE These files MUST be installed prior to the EDS application 2 Run the installation software Typically this installs the software automatically overwriting the previous version Some Internet connections have firewall protection which may prevent downloading of software from the Internet If you have difficulty downloading the software from our web site please contact your network manager to acquire the access rights necessary to download Administrator rights may also be required on the computer IXRF Systems Inc Iridium Ultra Software User s Manu
63. e the Sum Peak removal may not be selected In this case the button for Remove Sum Peaks will not be enabled after Remove Escape Peaks Instead it will be the Remove Background button 4 10 7 Background Modeling As an alternative to the automatic background removal the background can be removed from a spectrum by modeling the background from specific regions of the spectrum that contain only background no peaks These regions of the spectrum are selected by the user and can be stored in a file for use in processing the background of other spectra To access background modeling select Utility Model Background from the menu A dialog similar to the following will appear Backg round Model i Ciga Region Low High In modeling a background the spectrum iS broken up into eV ke discrete regions within which a linear or quadratic curve fit is done to model the background in that region Painting one or more windows on the spectrum creates a region in the background Use the spectrum window painting to define a region One would typically do this from left to right in the spectrum starting with a low energy region If you are unfamiliar with painting windows on the spectrum refer to the section on window painting in the chapter Working With Spectra This is an example of a region that has three windows painted After painting the windows press the Add Region button This wil
64. e of the detector window Working Distance This is the distance between the bottom of the objective lens pole piece and the sample Fixed Distance This is the vertical distance between the bottom of the pole piece and the center of the detector surface Tiltl Tilt2 10 0 1 These are the angle between the sample plane and the horizontal Azimuthal Angle This is the angle between a horizontal projection of the sample detector axis and a horizontal line defining the direction of tilt Detector Axis Angle This is the angle between the axis normal to the detector and the horizontal Detector Offset This is the distance between the detector window and the detector crystal measured along the axis of the detector Detector Active Area This is the active area of the detector in square millimeters Alpha Angle 56 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 This is the angle between the Take Off angle and the detector axis This parameter is calculated by the software Incidence Angle This is the angle of the electron beam with respect to the sample plane This parameter is calculated by the software Elevation Angle This is the angle between the detector axis and the horizontal plane This parameter is calculated by the software Take off Angle This is the angle of the analyzed x ray beam with respect to the sample plane This parameter is calculated by the software Detector Solid Angle This is
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66. ed or a default Au coating can be used Au 20nm thick The density of the coating can be entered or the Use Default option can be selected to always set the density to an internally generated value This coating information once entered will be used for the next ZAF analysis of the spectrum 4 10 5 Customizing Report Output The displayed and printed output from quantitative analysis Properties IXRF Calibration Std 2 can be customized This is done with the Display tab of Se the Spectrum Properties To access this select Properties from the menu and then click on the Display tab A dialog A similar to the following will appear Mass Thickness and Material Classification control whether these values are displayed Material Classification is discussed in a separate chapter in this manual Selecting Pie Chart will enable display of a chart of the analysis There are 3 primary tables of values which can be printed Components Table Elements Table and Conditions Table Clicking on these buttons displays the dialogs shown below which allow you to select the values that you wish to display Edit Component Display Yalue Display Numeric Precsi Component Type Mole Cone C 3 The Components Table as 7 Setup is normally used only if you wish to display the composition of the spectrum in stoichiometric form Normally only the elemental composition is displayed as setup in the Element Table Setup below When stoic
67. ed during the fitting Usually this kind of fit is adequate It is however important that the spectrum energy calibration is correct and the FWHM be set correctly Relative peak heights within a series e g Ka Ka KB KB for the K series are taken from tabulated values and are not allowed to vary during the fitting This means that if there are large absorption or enhancement effects in the sample this kind of fit will not perform as well as the non linear fit Non Linear Fit This fits the peak heights positions and widths to the spectrum This is a non linear fitting process because these variables are not directly solvable by standard linear least squares fitting Standard non linear algorithms are employed such as the Marquardt Levenberg method which allow the three parameters for each peak to be adjusted independently However in order to make this method work well for x ray spectra it is mandatory to include constraints in the fitting process The obvious constraints are 1 the relative line ratios for each line series that is fit 2 the expected allowable deviations of peak widths and 3 the expected or allowable deviations of peak positions The relative line ratios are reasonably well known but they can change depending upon the following factors a the overvoltage kV b the sample thickness and take off angle and c the composition of the sample In the latter case these may be absorption edges of other elements be
68. eese 128 10 5 1 Intensities OF Concent ations iscees en ceer cided ah ces coke Steed seedenite me EA EAEE EEEE EEKE E Eri 129 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 10 5 2 Oea On a oe eee ee emer ene N err Ory twaee tere try eT meter eter 129 10 5 3 Export Print and CN pb and ssiteticccstisc i E E A ES 129 TOG sii eT eSCanSystc 8salatecasaeaees E S 129 10 6 1 Sinclie Pace Output iy lessee esti aac o ate eek oicie ra eestiastadateea e eas 129 10 6 2 M h Page OUMU aaeeeecrree te rnens Ure wr E rey eee Tere ts tienes Teesret ee Vere een neni 129 11 WODO SARC E EE AE aca E E E E E E ec IEE wed E E E IRETE T E A 130 12 Stitched Images and Stitched Maps cccccccccccccsscsscsssccsssssssscsscsccsccccsssssssssssssssssssssssscsssssesecs 132 Pak AC Oee e r toe nc oa dete So aban ge ease ecto 132 2 Me CTIA ey tas ag esate tracers tsee ade te scta a ode cteso mecca ea a a se secteaees 134 B3 SAVING AnH EX POTN 2o sais eaenceestncnadica ye a oduiebtetaantadveeeuRtceees 135 13 WDA SUDDO ene na nna a EMER EA DEA OREN ES RN ERA DEA AMOS a EAPREDADEAMPEPEN SEE O PANE 136 14 Ber oy CUT GN os assoc dsc ee cd E A ecees 137 14 1 Omet DAC Cahbravion Model 500 OMY Vicia tarsus sanatce lions etautdsetenncuns eadabhiss bveceuatentdanteetsons cet 137 14 2 Manual Energy Calibration and Threshold Adjustment 1 0 0 0 cccccssssssseeeseeeeeeeeeeeeeeeeeeeeeaas 138 45 automatic Perey Cali Paton eese E E E i 140 hea sMOWws B
69. en the button text returns to Start the calibration is complete EE wiz wl 4 i E 140 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 14 4 Low Energy Calibration Low Energy Calibration can be used to calibrate the low energy portion of the spectrum On some systems it has been noted that the p peaks for light elements G e carbon and oxygen Automatic Manual Advanced FWHM Low Energy Calibration appear shifted in the Expected Out vs Measured In spectrum even though the higher energy peaks i e aluminum and copper are in their T correct positions To 1 0 i a we He a Enable Delete Fi ances ae isaseid o 0l 02 os 06 07 osi iab Low Energy a Calibration tab is provided in the Energy Calibration panel as shown to the right Expected Measured Energy keV Energy keV Low Energy Calibration can be enabled for each of the time constants For digital electronics it is practical to enable calibration for time constants 32 16 8 and 4 microseconds Shorter time constants are not normally used for light element detection To calibrate and enable the Low Energy Calibration for a time constant do the following Select the time constant This can be done from the Manual or Automatic tab of the Energy Calibration panel Ensure that the normal energy calibration is correct You can do this by acquiring a spectrum with two known elements in it
70. ensure that the deconvolution and quantitation parameters for any added elements analyzed e g C O are correct For light element detectors these low energy peaks can be analyzed and it is important that the deconvolution and quantitation parameters are set properly Elements that are below the Lowest Z Analyzed see Quantitation tab must be determined by stoichiometry To change the deconvolution click on the Decon method for the element in the Elements Analyzed table 42 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 Then select the desired deconvolution method Do the same for the quantitation by clicking on the Quant for the element and selecting the desired quantitative method For an easier method of dealing with oxides refer to the section 4 10 2 1 below A Type can be set for each component These are e Calc This is the most common type of component default This kind of component has its concentration calculated directly from the net peak intensities e Fixed These types of components have a pre determined concentration The concentration is entered in the Conc column During quantitation these component concentrations are fixed This can be useful if part of the composition of the sample is known e g H2O in CaSO 2H 0 e Diff This type of component assigns all of the remaining composition of the analysis to this component The total composition is the value specified in the Normalize Total defaul
71. ent any pixels with 108 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 counts below the threshold will be excluded from the Composite To change the threshold for an element click on the threshold column of the table in the row of the element you wish to change The histogram will appear for the selected element You can modify the threshold for the element as described in the section View Histogram Overlay Settings are identical to those found on the Element Selection tab of the FastMap properties Refer to section 9 3 on page 96 for details The composite map can be exported to a graphics file printed or copied to the Windows clipboard 9 10 Element Quantitative X ray Maps Individual element x ray maps calculated from quantitative analysis on the maps can be generated Acquire Clear File Edit View Process Create Quantitative Element Maps l Create Quantitative Component Maps Properties Sot sae Display Processing Whole Spectra Map Intensities Use Quick Linear Gauss Whole Spectra processes the spectra for each pixel in the map Full spectrum processing is performed This is the recommended option Map Intensities uses the map intensities directly in the ZAF corrections No background or overlap corrections are performed Use Quick Linear Gauss enables an optimized linear Gaussian deconvolution This option can be used for most maps and significantly improves the spee
72. ented to allow you to select which calibration value to use as shown below After completing the calibration the Calibration File Viewer will display the contents of the calibration file Below is an example of a calibration file Calibration File p Element Line Coefficient Coefficient a k Incidence Takeoff Standard Error 1 90674e 011 3 24219e 010 0 0151 1 99666e 011 8 05654e 009 0 2098 1 9067 1le O011 4 94711le 010 0 0181 1 996 74e 011 5 33025e 009 0 7569 Moxtek APS 3 63 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 It is important to verify the detector geometry and kV displayed It is a common mistake to have incorrect data in these fields This will lead to incorrect calibrations and poor quantitation using this calibration file Also note that this viewer can be invoked from the ZAF calibration panel using the View Calibration File button as shown below 4 13 4 Performing ZAF Quantitation with Standards After doing ZAF calibration quantitative analysis can now be performed using this calibration file If you saved the Analysis Settings from the ZAF calibration these can also be used as a good starting point for setting up the analysis From the Spectrum Properties dialog click on the Load Settings button and select the Analysis Settings file that you saved from the ZAF calibration Now from the Quantitation tab of the Spectrum Properties click on the Advanced button A dia
73. eps to elements with higher Z than a given element Elements below the given Z are processed using any stoichiometric information given in the components for the quantitation After deconvolution the Quantitation is performed e g ZAF Match which produces the composition analysis of the spectrum Select a method from the Quantitation Method list For standardless ZAF analysis no further setup is required For ZAF with standards or Match analysis an additional setup and or calibration step is required These methods are discussed in separate chapters in this manual The output of the quantitation is displayed typically as element concentrations however the composition can also be reported using stoichiometric compounds e g oxide or carbonate Stoichiometry is discussed later in this chapter The Excitation kV is displayed and can be modified It can also be estimated from the background in the spectrum The Duane Hunt method is used to estimate the kV if this is selected It can be especially useful if a sample is charging For charging samples the kV of the microscope may be considerably higher than the effective kV on the sample Apply kV to is used to change the kV of other opened spectra to the Excitation kV This can be useful if several opened spectra need to the same kV modification Material Classifications can be applied to the spectrum after quantitation This is described in section 4 16 4 IXRF Systems Inc Iridiu
74. er to make changes to that area You must click Apply or OK for any of your changes to be saved once the dialog is closed 3 6 3 System Setup Options This tab contains software options that can be enabled Enable VP Quantitation For systems that have variable pressure columns enabling this option will allow for the File New menu item to display VP Mode Spectrum Refer to the section Working with VP Spectra for details Enable XRF Software Options For systems that have XRF sources installed enabling this option will display the XRF specific controls in the software Enable Remote Control of XRF Tube For systems that have an XRF tube installed a serial interface can be used to control the tube This option enables the remote control of the tube Prompt to Save File when Closing Window Selecting this will enable Data Protection when closing files Refer to the section Data Protection 22 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 for details Prompt for save on Re Acquire of Data Each of these selections allows enabling of the Data Protection when acquiring data Refer to the section Data Protection for details 3 7 Window Menu The Window menu is shown below All of these menu items are common to Spectra Images X ray Maps and Linescans Window Help Cascade The menu items listed below Arrange Icons are special These menu Tile items are numbered 1 2 3 etc and ha
75. er will be prompted to save the data Whenever acquisition is started on a window that has previously acquired and not saved data the user will be prompted to save the previously acquired data These data protections can be enabled or disabled from the System Setup Options panel To access this panel select Tools System Setup then click on the Options tab A panel similar to the following will appear 24 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 4 Working With Spectra Right Click Menu File Edit View Acquire Analyze Overlay Utility Properties 6 Cursor 6 595 keV 7716 cnt ID Fe ka Fekal 3m lb6 Vart 10000 Window 0 005 40 955 495 271 ent Cursor Position Element ID Buttons Vertical Scale Spectrum Integral Shown above is a spectrum window As with all EDS windows e g Spectra X ray Maps a menu is available by clicking the right mouse button when the cursor is positioned over the window Shown above is the Right Click Menu for the spectrum Below the spectrum data is an Energy Scale This is used to interpret the energies of peaks in the spectrum To examine the energies of the peaks more closely a spectrum Cursor is displayed by clicking the left mouse button when the cursor is positioned over the spectrum The Cursor is a vertical bar on the spectrum as shown above The Cursor Position is displayed which includes the energy of the curs
76. eriodic Table method is especially m Cm Bk Cf Es Fm useful when identifying L and M series 4 7 3 Scrolling Peak Identifier It is possible to scroll through the periodic table using the Scrolling Peak Identifier To use this functionality select Enable at the bottom of the dialog Use the scroll bar provided to scroll through the atomic numbers The present element is displayed to the right of the scroll bar colored yellow on the periodic table and marked on the spectrum To add this element to the selected elements click the Add button When you have finished adding the last element be sure to uncheck Enable so that an unwanted element isn t accidentally labeled lines in the spectrum Co Ni Cu Zn Ga Ge As Se Br Kr d Ag Cd In Sn Sb Te I Xe Au Hg Tl Pb Bi Po At Ra Gd Te Dy Ho Er Tm Yb Lu Hide MLK Markers 33 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 4 7 4 Cursor Identification A list of the possible peaks at the Cursor energy is displayed below the spectrum This is the Cursor ID list Double clicking on an element on this list adds or removes the element from the manually identified element list Ci
77. ermine this drift by acquiring digital images during the map acquisition and tracking the change of position of a feature in the image Enabling drift correction for x ray maps does this Normally x ray maps are acquired using the full scan range of the our electronics This acquires a map that corresponds to the full image of the microscope When drift correction is enabled a border region around the full image is reserved for any drift corrections that may be necessary during the map acquisition The panel below shows a digital image and the border red rectangle The map will acquire data inside the rectangle labeled Map Scan Area This will allow for the sample to drift horizontally and vertically by the distance outside the rectangle Select Pattern on Image for Drift Tracking Define Use Current Default Map Area Map Area Map Area Select Test Pattern on Image Selected Patten This must be smaller than the full scan area to allow for drift corrections Cancel 120 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 9 18 1 Enabling Drift Correction To begin using drift correction check the Enable Drift Correction setting on the acquisition panel of the properties for x ray maps as shown on the right 9 18 2 Acquiring Maps with Drift Correction With drift correction enabled whenever an x ray map is acquired the following panel will appear 121 IXRF Systems Inc Iridium Ultra So
78. ertical Scaling is available from the menu as View Auto Vertical Scale and also as the ToolBar button When this feature is enabled the spectrum is scaled vertically such that the tallest peak in the window scales to the top of the window 4 2 3 Manual Setting of Displayed Energy Double clicking on the Energy Scale displays a dialog to manually set the energy scale Displayed Spectrum Energy This allows for setting an exact energy range for the display of the spectrum Often when preparing to print MT keV to 20 005 keV SetasDefaut a spectrum it is necessary to adjust the displayed spectrum to show a specific energy range This is sometimes difficult to achieve with the Cursor Enter the energy range that you wish to display in the spectrum window This panel can also be used to set the default energy range used when displaying spectra In some applications it is only necessary to view spectra from 0 20 keV In cases like these you can enter the energy range as 0 20 and then click on Set as Default This will ensure that all subsequent spectra will have an initial display of 0 20 keV It will still be possible to view the data above 20 keV but the initial display will always be O 20 keV cance 4 2 4 Bipolar Display Bipolar display of spectra shows both positive and negative channel data Normally a spectrum does not contain negative channel data An exception to this
79. etails on setting the threshold Show Map If this is selected the element will have a separate panel displaying the element This is set by default if the display mode is Individual Maps Display If the display mode is Overlaid Maps Display selecting this option will display a separate panel for this element On SEM 97 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 If this is selected the element is overlaid on the SEM image This is set by default if the display mode is Overlaid Maps Display If the display mode is Individual Maps Display selecting this option for the element will overlay the element on the SEM image The Element Settings table allows you to modify which elements are displayed as individual maps Display Map or overlaid on the SEM image Overlay Map Thresholds for each element can also be selected by clicking on the Threshold column for an individual map The map histogram is displayed and a threshold can be set for each element Overlay Settings control how the overlaid maps are displayed A filter can be applied to the maps A Gaussian Smooth or Median Filter can improve the appearance of the maps The size of the filters can be controlled larger values produce a more pronounced effect on the maps Auto Color Leveling can be applied to the maps as well Transparency controls the combining of the maps with the SEM image The combination can be controlled from opaque maps no SEM image visible t
80. ettings on the SEM image 9 5 View Histogram Histograms for each element can be displayed with the View Histogram menu item or on the Element Selection property panel for the FastMap Shown below is a histogram for Fe Sample f Histogram Fe WwW Threshold The histogram display has a colorbar green in this example at the bottom showing the correlation between intensities and color in the map Each map has a threshold setting for display Initially this threshold is disabled so all intensity levels are displayed in the map and overlay Sometimes it is useful to display only a given range of intensities for example to exclude very low levels of intensity To enable a threshold select Threshold as shown above When first selected the threshold is shown as the full range of values in the map Using the slider you can select a minimum threshold for the intensity The values displayed are colored yellow in the histogram As the user modifies the threshold the map and overlay on the SEM image are updated 102 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 9 6 The Sum Spectrum and Maximum Pixel The Sum Spectrum records all x rays that have been acquired during the map acquisition thus it is the sum of all x rays from all pixels in the map The Summation Spectrum is sensitive to the dominant features of the data cube The Sum spectrum is always available in the display area below the maps as shown below
81. for an element The Oxide is restricted to the element oxygen The Reset selects the default oxides for the selected element The Reset All button restores all elements to their default settings 4 10 3 Minimum Intensity Criteria Minimum Intensity critiera can be used to eliminate those elements from the quantitation whose intensity is less that a given number of standard deviations of the error in the intensity This can be useful when the presence of an element is not known prior to quantitation This is especially useful when standardless ZAF corrections are being used This option is found on the Advanced quantitation panel From the spectrum Properties panel click on the Quantitation tab then click on the Advanced button On the Advanced settings panel select Apply Minimum Intensity Criteria as shown below After the deconvolution processing the intensity for each element will be tested Elements whose intensity is less than the allowable value will not be included in the quantitative analysis 4 10 4 Sample Coating and Thickness Provision for including a sample coating is provided This can be useful in improving ZAF quantitation To define the sample coating select Setup in the Coating section of the Advanced Quantitation settings of a spectrum A panel similar to the following will appear 44 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 Sample Coating The coating element can be enter
82. ftware User s Manual Rev 1 4 Select Pattern on is for Drift Tracking x es Define Use Current Default Map Area Map Area Map Area Select Test Pattern on Image Selected Patten Stop if sample drifts out of range Instructions Select the Map Area This must be smaller than the full scan area to allow for drift corrections Cancel A digital image will be acquired Instructions for setup are displayed in the lower right corner of the panel The first step is to select the map area This is the actual area for the x ray map It must be smaller than the full image area so that our electronics can make adjustments to the beam positioning horizontal and vertical to accommodate for the drift There are three options for defining the Map Area 1 Click on Define Map Area This allows you to select a rectangular area on the image This area will be the actual area that the map will be acquired over The remaining image area will be used for drift correction 2 Click on Use Current Map Area Displayed on the image is the Map Scan Area that was used for the previous map with drift correction If you wish to use the same map area select this option 3 Click on Default Map Area This selects the system default map area 10 border on all sides After selecting the map area you will need to select a pattern in the map area that the drift correction software will use for tracking movement Select a feature on the image that is lo
83. g will appear Select the type of file desired Create Analysts Data Combined SEM AF Image Fast Map Fast LineSican Spectrum Report Least Squares Calibration Stages can Stage Map Stitched Images Stitched Maps YF Mode Spectrum 3 4 2 Open Opens one or more previously stored Spectrum Image EMSA format spectra files etc from disk To open multiple files use the control and shift keys as with common windows list selections 13 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 3 4 3 Save EDS Data Set Saves all opened EDS data to an EDS data set file so that data from an analysis may be logically grouped together in a single file 3 4 4 Set Sample Name Allows for setting of a sample name A panel similar to the following will appear The text entered as Sample Name will be used to name all subsequent data acquired in the software e g spectra images maps linescans In the above example the data are given names of XRF Calibration Std 1 IXRF Calibration Std 2 etc The Preset Index is the current number that is suffixed to the Sample Name In this example 2 is the next number The index can be reset to restart the suffix to 1 if desired by clicking on the Reset Index button The present Sample Name is displayed on the application status bar at the bottom of the application window as shown below Foe Computer w A RichLamb g Libraries ae
84. h Samples After entering the materials it is important to verify the classification on some representative samples Start by saving the Analysis Settings which now include the enabling of the Materials Classification and the names of the Database and the Materials Class that are to be used Acquire spectra from the samples and perform quantitative analysis on them At the bottom of the quantitative analysis will be displayed the material which matches the quantitative analysis If nothing is displayed check the setting in the spectrum Properties Display tab Make sure that Material Classification is selected as shown Acquisition Element ID Quantitation Display Spectrum Display Display and Print Settings Quantitation Display Hements Table Conditions Table Mass Thickness 83 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 4 16 6 Setting Minimum Counts in Spectrum It is possible to set a minimum threshold for counts in a spectrum This eliminates a spectrum from classification if the total counts in the spectrum are below a minimum value This is set in the Material Classification setup panel The setting of O for Minimum Counts as shown will effectively not eliminate a spectrum from classification Setting this to a value above 0 will impose that limitation 4 17 Spectrum Simulation CAISRFOAT A Input mdb Spect
85. h keV display the x ray energies used to construct the linescan for each element In the example above the Si linescan is constructed using the Ka line series x rays of Si which correspond to energies between 1 691 1 789 keV If a different line is selected for an element the Update Graphs button must be pressed to apply the changes to the linescans By default the element ROIs for maps and linescans is 1 8 FWHM around the peak center Below is an example of the ROI for Fe using one FWHM By setting the ROI Width to 2 0 most of the peak area is included in the map for Fe as shown below 10 4 Viewing Intensities and Concentrations E Element Inteneities Concentratione EA Select View Intensities Concentrations from the menu to E inspect the x ray data at individual points on the linescan This panel will appear Click anywhere on a linescan to select a point to inspect the x ray intensities as shown below 126 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 The panel now displays a histogram of the intensity of each element at the selected point Selecting Concentration in the panel will apply ZAF corrections to the intensities and re display the histogram with these calculated values in weight percent as shown here Note All points on the linescan must be quantified during this process This may take a considerable amount of time A progress panel will appear with a Cancel b
86. hat the complete Cr 20 983 wt description of the standard is entered into the Mn 1815 wi component table You can start with the default list Fe 75 688 produced by the standardless analysis but you must make sure to enter any other elements present in the standard though they may not be selected for calibration This is extremely important To generate the correct values for calibration coefficients the ncentration Total 100 00 wt complete sample composition must be specified otherwise incorrect calibration coefficients will be generated Itis also possible to enter compounds directly in standard e g oxides or carbonates In these cases the unanalyzed elements e g H or C will be determined by stoichiometry As you enter the assay values in the component table they will appear in the Element table at the bottom of the dialog When you have completed the entry of the assay Conc 1514 20 983 L815 75 688 Hall Quantitation Units wt wt wt wE to UnAnalyzed Fraction 4 00 values click on the Save button to save the standard file The same name as the spectrum should be chosen for later use in the calibration step Do ZAF Calibration View Calibration File Select Utility Quantitation Calibration from the menu A dialog similar to the following will appear If the Standard file name that you wish to use is not listed in the field to the right of File click on the Browse butt
87. he automatic background setup parameter Filter Width controls this filter width that distinguishes the peaks a larger width parameter would be more suitable for wider peaks Iterations controls the number of repeated operations too low a number may result in an over estimate of the background Reset to Defaults will restore the values of Iterations and Filter Width to factory settings After the preliminary spectrum processing is complete the net peak intensities must be calculated In the software this step is referred to as Deconvolution because of the need to correct for peak overlaps Two methods are provided for deconvolution Gaussian and Integral Gaussian is the most common method This method fits theoretical Gaussian shaped peaks for each specified line in the spectrum which takes into account peak overlaps such as Ti Ka with Ba La A complete discussion of Gaussian deconvolution is given later in this chapter The Integral method of deconvolution merely calculates the sum of the counts in the peak regions of interest ROIs in the spectrum This method works well if there are no peak overlaps in the spectrum However since the Gaussian method works well in all cases it is preferred Lowest Energy Processed is used by Background removal and Deconvolution to limit these processes to spectral data above a given energy Lightest Analyte is used by Deconvolution and Quantitation to limit processing of spectral data in these st
88. he beam current for the unknown samples can vary but still the beam current for all the standards must be the same The geometry must also be the same e g same working distance Therefore the user should make the trade off between simplicity of use vs potential accuracy of analysis 59 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 4 13 2 Calibrations ZAF quantitation using good quality pure element or type standards will often yield more accurate results but the user must take more precautions As in any quantitative analysis the quality of the standard is critical to getting reliable results For SEM EDS analysis the surface condition is very important especially for light elements 1 e low energy x rays At about 1 keV the x ray signals come from the top 1 micron of the sample with a large fraction coming from the first tenth of a micron Because of this surface sensitivity that is even worse at lower energies the specimens should be polished to a local flatness of lt 0 1 micron for x ray energies at 10 keV a 1 micron polish is sufficient Of course the specimen must be globally flat as well over the complete surface area but this can vary by several tens of microns without any serious problem One of the advantages of ZAF or other quantitative method calibration with standards is that many of the primary fundamental x ray parameters are eliminated from the calculations In particular the
89. he detector is not a chisel nose The setup of these detectors only requires entry of Tilt Detector Axis Angle and Azimuthal Angle Refer to the section 4 11 1 fora description of these parameters For off axis detectors the full set of geometry parameters must be defined Any information from the detector manufacturer regarding the geometry will be very useful in defining these parameters Refer to section 4 11 2 fora description of these parameters Properties IXRF Calibration Std 2 Acquisition Element ID Quantitation Display _ Number of Smooths 1 Remove Si Escape Peaks Remove Sum Peaks Lowest Energy Processed 0 100 Background Method Auto Setup The diagram below describes the geometry of the EDS detection system in an electron microscope The geometry is Deconvolution conceived as a eucentric stage pivoting about the impact point Method Gauss 7 Setup of the electron beam on the sample Tilt1 and Tilt2 are orthogonal axes of tilt and Theta is the number of degrees of rotation The Azimuthal angle is the degrees of rotation of the detector axis about the Tilt 1 axis and the Elevation is the angle between the sample plane and a line that intersects the center of the front of the detector The Detector Axis Angle is the angle between the detector axis line and the horizontal plane The Working Distances in mm is the distance between the analys
90. he noise peak disappears 139 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 14 3 Automatic Energy Calibration Automatic Energy Calibration performs fine adjusts the Gain and Zero of the DPP to achieve optimal calibration of the energy scale of the spectrum Acquiring a spectrum with known peaks in it and then automatically measuring the energies of these peaks performs this From the measured and known energies of the peaks adjustments are made to the Gain and Zero of the DPP This process is repeated until the known peak and the measured peak energies agree to within the desired tolerance Click on the Automatic tab of the Energy Calibration panel to access the Automatic Energy Calibration A panel will appear as shown here The power on the DPP should be turned on for at least one hour prior to performing this Automatic Manual Advanced FWHM Low Energy Calibration AlCu j Low 1 487 keV calibration If the power is off turn on the power and continue Tolerance 0 003 keV High 8 041 keV with this calibration after one hour Preset 30 as SE o o Peak Center _ The known peaks for the Calculate am E calibration are selected from the list in the upper left corner Shown in this example is the AlCu sample This sample has an Al ko peak at 1 487 keV and a Cu ka peak at 8 041 keV These are displayed as the Low and High peaks in this example If Al Cu is used note that the Al
91. hiometry has been setup for the analysis it is common to select Component Concentration and Units Numeric Precision is used to j adjust the output of values For example by default concentration displays with 3 digits i e 45 127 Laad settings Changing the Numeric Precision to 1 for concentration will display 45 1 The Mole Concentration expresses the composition in terms of a molecular basis where each molecule corresponds to the compound molecular formula This is analogous to atomic concentration see below 45 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 The Element Table Setup allows for selection of the values displayed for each of the elements Typical selections are shown which display the element line intensity concentration and units for the concentration Detailed reports can be displayed which contain estimates of background intensities calculated MDL minimum detection limits etc Note that Numeric Precision can also be modified as described for the Component Table above ORMOOUOOUOUOUOUROOOURO The Condition Table Setup allows for display of acquisition processing and match analysis values For ZAF quantitation kV is typically selected along with the spectrum processing parameters and the livetime For Match quantitation Best Match Spectrum and ALL Matching Spectra are typically selected Note that Numeric Precision can also be modified as described for the Com
92. i 350 c Fe i sf ed ee Cursor 8 305 keV 258 mt ID Yb b4 Ekg Ato Vert 7000 Window 0 005 40 955 922268 at Elapsed Livetime 1000 aj Preset 100 Mode Time 0846 Et Lire itensiy Eror Quart Atomic Cone Eror Eke BkeEror MDL icis 2 sig Ys 2 sig Ttic s 2 sig 3 sig 000 0000 Ato OOOO 0O00 wti 0000 161 0254 0000 5950 1543 Auto 0559 0465 wt 0012 563 0475 000S 4256 1305 to 0416 0363 wt 0011 1085 0659 0012 888440 18351 Auto 89033 84 119 wt 0 178 1536 0734 O016 64956 5097 Ato S667 5510 wt 0043 1362 0738 0014 4967 1410 Auto 2814 4967 wt 0 141 232 0305 006G 060 0155 Ato 0059 O106 wt 0027 162 0255 0098 8109 1801 Auto 1451 4470 wt 0099 183 0271 0032 100000 100000 wt Total 350 Tikeof Angle 350 a 10 15 Esc On auaa Oe ee a Smooth 1 Cursor 8 035 key 51554 at ID Cuka Tm b4 Fill Cukal Ho b5 Ekg dto Vert 1000 Window 0 005 40 955 1233435 at Elapsed Livetime 1000 7 mi pil Guss Fit 5477 89 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 7 1 Acquiring Spectra Each of the spectra must be acquired separately Click on the Acquire button on the toolbar A panel similar to the following will appear Select either SEM or XRF and pressing OK will start acquisition of the spectrum Prior to acquiring the spectra be sure that the proper beam is turned on SEM beam for the SEM spectrum XRF source for the XRF spectrum To acquire the SEM spectrum make sure that the XRF source is turned off
93. ically for the kind of window e Update the status of the ToolBar buttons Only the buttons that apply to the active window will be enabled all other buttons will be deactivated and will be displayed grayed out An example of a disabled button is seen on the far right side of the ToolBar The button is not active for the spectrum window 10 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 3 2 ToolBar The ToolBar contains buttons to perform common tasks and displays status information during spectrum acquisition Below is a brief description of each item on the ToolBar Prints the active window Displays information about the software Creates a new active window e g Spectrum Image Opens a previously stored Spectrum r Image etc from disk Stores the active window Spectrum X ray Map etc on one of the system s disks Creates a new combined SEM XRF spectrum Copies the active window e g Spectrum Image to the Windows Clipboard Creates a Fast Map using the element list of the spectrum and start acquiring the Fast Map Creates a new spectrum and start acquisition of the spectrum Closes all opened windows Creates a new Image and start acquisition of the image F Creates a Fast Linescan using the element list of the spectrum and start acquiring the Fast Linescan Toggles Spectrum Auto Vertical Expands the spectrum Vertical Scale Scaling Contrac
94. ids and coatings see below Window Thickness This is the detector window thickness in microns Window Coating Material Many windows are coated with a thin layer of some element to prevent light from entering the detector which would result in large amounts of noise in the spectrum and poor resolution For Be windows no coating is required but ultra thin windows almost all require some kind of exterior amp sometimes interior coating The default window coating element is aluminum If no coating exists just set the thickness to zero and the window material element will be ignored Window Coating Thickness This is the thickness in nanometers of the window coating Carbon Contamination Often after extensive use or a leaky vacuum system diffusion pump oil may be deposited on detector windows as this is often the coldest part of the vacuum system The carbon contamination parameter is an estimate of the thickness of this oily contamination layer to help obtain reasonable standardless analysis under these circumstances This oily layer should be removed carefully by a qualified service technician Support Grid Thickness Many windows are too thin to be supported across the width of the detector opening In these cases a grid is used under the window to provide the support with a pressure differential from air to vacuum The grid material is usually implicitly specified as part of the window type see above and may or may not be
95. iers y C abr OM sxca was ai saneuics E EE E aa ia wea den E EE EETA 141 HES VOW IADU oun AEE E EEE E EAEE 143 o Calculate Detector FW HM earen E N EA T E E AE 143 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 1 Introduction Welcome to the EDS system from IXRF Systems Inc This combination of hardware and software is a powerful yet easy to use system encompassing all aspects of x ray microanalysis and optionally XRF X Ray Fluorescence Because of the technology used Energy Dispersive Spectrometry this technique is often referred to as EDS analysis The purpose of this software is to acquire and analyze X ray spectra x ray maps and linescans and electron images to perform a complete analytical analysis of a sample located in a Scanning Electron Microscope SEM or Transmission Electron Microscope TEM Operating on all of the current Microsoft operating systems Windows 2000 Windows XP Vista and Windows 7 the EDS software seamlessly integrates with many other powerful applications to provide custom report generation and connectivity with other networked systems The purpose of this manual is to describe the common activities that the EDS software is designed to perform As such the primary chapters are titled Working with It is assumed that you are familiar with the basics of operating a Windows application and that you are familiar with the common terms and techniques of EDS analysis If you are not
96. ile name Magnification This is the present microscope magnification Field Size Calculated from the magnification calibration in the EDS software this is the size of each image field This can be used to verify the calibration on the SEM prior to starting the stitched image map acquisition If there is a discrepancy between this field size and the SEM field size it is recommended that you do an image calibration prior to proceeding Stage This selects the stage that will be used for the automated operation Normally this is set to Microscope Stage However if you do not have an automated stage or if you want to manually position the stage you may select None from the list Upper Left Location Move the stage to the upper left location for the stitched images and click Set This will record the stage location At anytime you can click on Go To move the stage back to the upper left location This can be useful in verifying the area for acquisition Lower Right Location Move the stage to the lower right location for the stitched images and click Set This will record the stage location At anytime you can click on Go To move the stage back to the lower right location This can be useful in verifying the area for acquisition Number of Fields Horizontal This is the number of images horizontally in the stitched image This is calculated automatically when you select an upper left and lower right corner The automatic calculation can be change
97. ined Values larger than this add no additional information to the x ray map 95 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 Properties FastMap1 eres Multi Scan acquires multiple scans frames of the x ray map The frames are summed together producing ever increasing quality in the x ray map as the frames are acquired Max Scans 5 73 3 No F is the maximum number of frames that will be acquired The Na Me aan ake saal acquisition can be stopped at any time allowing the user to K Ca Sc Ti v Cr EAA co Ni Cu Zn Ga Ge As Se Br Ke i Rb Sr Y Z Nb Mo Te Ru Rh Pd Ag Cd In Sa Te 1 x determine when the x ray maps are of sufficient quality For eee EEE example a Point Dwell of 100 Sec and Resolution of 256 Ce Pr Nd Pm Sm Eu Gd Tb Dy Ho Er Ta Yo Lul square will complete a frame in about 7 seconds If Multi Scan ge ace pe is enabled and Max Scans is set to 500 the completed x ray map Remove All v Enable Quick Select WD will acquire a total of 50 mSec of data for each point This is Element Settings calculated as 100 uSec x 500 50 mSec The advantages of ROI Width 1 8 FWHM Restore Defaut ROI performing the x ray map with Multi Scan are QO The x ray map can be stopped at any time from 7 seconds to one hour the time to complete all 500 scans The a Naas ee a aaa ao hap user can select when the x ray map has sufficient quality 0 201 0 353 QO Sample charging effects are minimized d
98. ing diagrams of the relationships of the parameters refer to the section 4 11 above 55 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 Tilti Tilt2 These are the angle between the sample plane and the horizontal Detector Axis Angle This is the angle between the axis normal to the detector and the horizontal Click on the Change button to modify this parameter Azimuthal Angle This is the angle between a horizontal projection of the sample detector axis and a horizontal line defining the direction of tilt Click on the Change button to modify this parameter Incidence Angle This is the angle of the electron beam with respect to the sample plane This is computed by the software Take off Angle This is the angle of the analyzed x ray beam with respect to the sample plane This is computed by the software Detector is on axis This allows for changing the detector from on axis to off axis For a description of these terms refer to Detector Geometry 4 11 2 Off Axis Detector Geometry n m m This panel is used to define the detector geometry for systems that do not have an on axis detector This panel allows you to set all parameters that describe the geometry For a complete discussion of these parameters including diagrams of the relationships of the parameters refer to section 4 11 am mm uo on i Horizontal Distance This is the distance between the sample and the fac
99. ion methods Change all element quantitations to Auto 90 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 To quantify the combined spectrum right click on one of the spectra and select Analyze After quantitation the results panel will display the Combined Analysis Combined Analysis SEM and XRF Details Combined Analysis Elt Line Intensity Error Quant Cone Error cis 2 sig 2 sig gt Ea O 00 0 000 Nene O 000 wtta 0 000 Fe Ea S950 1 545 FP 0 693 wto O 018 Hi Ea 7 09 0 533 ZAF 0 252 wt o 0 019 Cu Ea 1 709 02 6 268 24AF 61 551 wt 0 595 n Ea 649 56 5 097 FP 6 526 wt 0 050 ei Ea 49 67 1 410 FP 5655 wto 0 166 wo Ea 0 60 0 155 FP 0125 wt 0 052 Fb La 61 09 1 801 FP 5 164 wta 0 115 100 000 wt o Total The Combined Analysis is a summary Combined Analysis SEM and RF Details analysis report It give the final elemental and SEM Aralysis component analysis of the SEM and XRF Et Lie lntersity Emor Chant Cone Error spectra Note in the example above that Ni oSI eels 4 818 and Cu were analyzed using ZAF and the i i ee ried nen es aah ane WET remaining elements by FP S was not a oie Sie foo ae ai analyzed due to zero intensity and is reported tf Ea 170902 8268 ZAF 81581 wht 0395 with analysis method None m Ea 0233 19223 Jute 0O00 wey o 000 Sr La W420 2042 wto 0000 whe O 000 For details of the SEM and XRF click on the ee see Hae aon nae SEM and XRF Details tab This displays the 51
100. is A panel similar to the following will appear T2 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 Select Standard s Look in LSDemo J t My Recent Documents Deskto m o E tx My Documents p PE My Computer i bly Network File name Places Files of type Standards std Cancel Select one or more of the standards displayed and click Open to add them to the calibration You may notice that some of your standard files std are not listed in the panel This is because there is not a spectrum file xsp for the standard file in this folder Standard and standard spectrum files must have the same name and be stored in the same folder in order to be used with LS calibration After selecting the standard files the calibration is immediately performed and graphs of the curve fits for each element are displayed The calibration includes all elements that are in the calibration standards Below is an example with 3 standards selected from the panel above 0 1 000 2 000 50 000 100900 150 009 73 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 The graphs are displayed with concentration on the vertical axis and intensity on the horizontal axis The intensities have been taken from the standard spectrum files from the last quantitation of each spectrum The concentrations are taken from the standard files The pairs of intensity and concen
101. is point and the detector crystal The Horizontal Distance is the horizontal distance between the front of the detector and the analysis point and the Working Distance is the vertical distance between the pole piece and the analysis point and the Fixed Distance is the vertical distance from the pole piece to the horizontal plane which intersects the center of the front of the detector The vertical working distance computed is the difference of the last two measurements and is the vertical distance from the front of the detector to the analysis position Derived from this geometry is the Incidence Angle of the electron beam with respect to the sample plane and the Take Off Angle of the analyzed x ray beam again with respect to the sample plane Alpha is the angle between this line and the detector axis line The Elevation Angle is the angle between the line through the detector axis and the horizontal plane Geom Osteo x 54 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 Top View of Electron Column Detector Detector Crystal Pole Piece Electron Beam Oh On 4o JA Fixed Distance Working Detector Distance Crystal Detector Sample Horizontal Distance 18 4 11 1 On Axis Detector Setup This panel is used to define the detector geometry for systems that have an on axis detector For a complete discussion of these parameters includ
102. ish and export the x ray maps 104 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 9 8 Viewing Intensity Composition of Points on X ray Maps Selecting View Element Intensites from the menu to inspect the x ray data of individual pixels points in the maps The following panel will appear Locations Locations Location Click anywhere on a map to select a location to inspect the x ray intensities at that point as shown below Locations Locations Location Cursor 73 402 um 39 232 pm The panel now displays a histogram of the intensity of each element at the selected point 105 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 9 8 1 Modes There are 3 active modes to view the x ray map data Spot Rectangle and Freehand These modes are described below along with the inactive Off mode The Intensity or Concentration selector determines the values that will be displayed in the histogram and the Locations list described later 9 8 1 1 Off Mode No interaction with the x ray maps This mode is set after a Rectangle or Freehand has completed and after a Save Spot operation completes 9 8 1 2 Spot Mode With the left mouse button pressed over an x ray map or the included microscope image the intensities or concentrations from the spot are displayed in the histogram If Show Spectrum is selected the spectrum for the location on the x ray map will be displayed below
103. ka peak must be larger than the Cu La peak If necessary change the area from which the spectrum is being acquired Also note that sufficient EHT must be applied to efficiently excite the Cu ka peak At least 20 keV is recommended Tolerance is normally set to 003 keV The calibration will continue to adjust the Gain and Zero until both peaks Al and Cu are within 003 keV of the known energies Preset is set in Livetime Seconds or Integral Counts This value overrides the setting in the spectrum during the automatic calibration If the count rate is less than 2000 c s it is recommended that the Preset be at least 40 seconds Longer Preset values will generally yield more accurate energy calibration Batch can be used to calibrate all time constants sequentially This can significantly reduce the tedium of the calibration process Select Batch prior to starting the calibration if this option is desired Click on the Start button to begin the automatic energy calibration If the Batch option was selected a dialog similar to the following will appear Select Time Constants J Select the Time Constants that you wish to calibrate and click OK to begin the calibration The automatic energy calibration can take several minutes to complete for each Time Constant During the calibration the status of the calibration is displayed and the Start button is replaced with a Stop button If you wish to cancel the calibration press Stop Otherwise wh
104. kgrounds but often the situation is not that simple For example in electron beam microanalysis EDS there are regions of the background that have relatively high curvature and there are often small noisy peaks superimposed on high backgrounds The background curvature arises from several effects including the deceleration effects of electrons in bulk solids which produce the characteristic bremsstrahlung x ray continuum whose shape depends on the sample mean atomic number and the incident electron energy microscope voltage in kV Superimposed upon this continuum are the absorption edges of both elements in the sample and in the detector and window The latter result in the steep low energy fall off typical in most EDS spectra These absorption edges are not visible as discrete steps in the spectrum because they are convoluted with the detector response function which results in the smearing of these steps The basis of the automatic background therefore is to filter the spectrum in such a way as to remove the sharper peaks leaves the smooth background which is subsequently subtracting from the original spectrum 40 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 Automatic Background Setup Clicking on the Setup button in the Background section displays a panel similar to the following Automatic Background Setup erations Ell Reset to Defaults Filter Width 200 00 0K Cancel T
105. l insert the painted windows into the list of windows A polynomial will be fitted to all the window channels within this region resulting in a model of the background 1 2 keV 47 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 Below is the result after pressing the Add Region button The background has been fit between the windows painted and these windows have been added to the list as erame Region 0 There are 3 windows in this region therefore a quadratic f ina will be fit to the region The energies in keV of each of the painted Delete Windows E o 0 735 0 825 windows of the region are displayed in the table as the columns Oera re ae labeled Low and High Subtract Open Save Fok Cercei Another background region can be defined and added to the model by repeating the above steps of painting background windows and pressing Add Region This is an example of this A new region has been added just below the previous region This new region is overlapped on the previous region This overlapping will ensure a continuous and smooth background model 1 2 keV Here is the result after pressing the Add Region button Notice that there are now two regions in the list Background Model This process can be repeated until a complete model of the ion i Region Low High keV keV background has been made for the whole spec
106. l of the linescans are fit to a single page of paper The image can be included on the page For portrait output the Printer System Printer Epson Stylus COLOR OK image is printed at the top of the page For Printing 2 ne landscape output the image is printed on the left side of the page IY Print Image MMultt Page Output Linescan Per Page 2 10 6 2 Multi Page Output Eo A First Page Only Even Fage Nolmage For this style you specify the number of linescans per page Thus if you have 8 linescans and print 2 per page the output will be 4 pages The image can be printed if desired on either the first page or on every page 129 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 11 RoboStage RoboStage allows unattended acquisition of multiple EDS data from anywhere on the microscope s stage using the existing stage automation for the microscope to position the stage for each EDS data acquisition Data are automatically saved in either individual data files or an EDS Dataset file Below is the main panel for RoboStage This panel is accessed from the menu item Tools RoboStage oe o a M Save Data Individual Files EDS DataSet Select Data to Acquire Stitched Images Stitched Maps StageMap Auto Focus Status Name Type Seid Settings Auto Auto Grid Grid x pecan Y mm File Focus B C Rows Cols Overlap LK 1 Image 65 884 23 016 500 LK 2 Spectrum 65 619 22 8
107. lays the material name View Stage Position Displays the stage location for each spectrum View SEM Magnification Displays the microscope magnification for each spectrum View Select Element Values 87 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 Allows for display of any Element values concentrations intensities etc View Select Component Values Allows for display of any Component values concentration type etc Data Add Spectra Invokes a dialog to Select Spectra for Report Data Delete Spectrum Removes the currently selected spectrum from the report When this is done the table is redisplayed Data Re Analyze Performs quantitative analysis on all of the spectra in the report and redisplays the report This can be useful if you wish to change any parameters of the quantitative analysis Using this menu item automates the re quantification of all of these spectra the table is redisplayed after the quantitation is completed 88 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 7 Working with Combined SEM XRF spectra With the addition of the fX and X Beam XRF sources to our product line it is now possible to analyze a sample using both e beam generated and x ray beam generated spectra Analyzing samples separately with e beam and x ray beam is straight forward using the standard spectrum acquisition and analysis tools Performing combined analysis using both spectra from a sample
108. log similar to the following will appear 5333 5497 ZAF 5 814 5983 ZAF 6317 6491 ZAF 7385 7 571 ZAF Select the elements from the Elements Analyzed table that you wish to quantify with the ZAF calibration file Normally this will be all of the elements To select all elements in the table do the following 64 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 Siena er left of an element name e g Cr kew j kev File GAUSS 5 336 5 494 Mone This selects a single element in the following example it is Cr e Further elements can be added by selecting their individual select buttons 336 Mone Mone e To select all elements in the table 3 ke w E o press Ctrl A on the keyboard Co Ka s 6845 7 015 None T 391 F565 Mone e Click on the Calib File cell of the table on one of the selected rows e g Cr A dialog similar to the following will appear which will wi steel pc allow you to select a ZAF calibration file Select a calibration file The file name will now appear for all of the selected elements as shown here File name a Files of type ZAF Cal Files fpc Cancel Open as read only we e To unselect the complete table now press Ctrl E on the keyboard Note that each element may be quantified by a different calibration file e g if each one had a separate pure element calibration file steel fpe isa A Me 5 1 GAUSS Bi 47 TA
109. ltra Software User s Manual Rev 1 4 4 15 2 Quantifying with Least Squares To use Least Squares for quantitation you must select LS as the quantitation method and an appropriate LS calibration file for the desired elements LS quantitation selected from the Quantitation tab of the spectrum Properties panel as shown below 11 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 Click on the Advanced button in the Quantitation section A panel similar to the following will appear 0 000 0 000 wt 0 000 0 000 wt Gauss 6317 6 491 ZAF wt Gauss 6 840 7 020 ZAF wt Select the elements that you want to analyze with LS Change the Quant method to LS by selecting LS from the list of quantitation methods as shown below Fe Ea l Gauss Zz Co Ka Gauss Then click on the Calib File column for the element A panel similar to the following will appear for selection of the calibration file 78 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 Select Calibration File 7 Look ir LSDemo My R sacl Documents Deskto m Least Squares Calibrationa My Documents wr a My Computer l biy Network File name Places Files of type Least Squares Calibration lsc Cancel Select the calibration file and click Open The spectrum is now setup to quantify using Least Squares You can save these settings for use with other similar
110. m Ultra Software User s Manual Rev 1 4 4 10 2 Using Stoichiometry Oxides etc If the desired output is to use the stoichiometry formulae for the analysis of the sample you must enter the compound stoichiometries prior to the analysis This is done in the Advanced dialog for Quantitation To do this access the Analysis Settings as described earlier in this chapter and click on the Advanced button in the Quantitation section of the dialog 2246 2370 ZAF 5 333 3 497 ZAF 5 814 5 983 ZAF 6317 6491 ZAF 7 385 7 571 ZAF The stoichiometry of the sample is entered in the table at the top of the dialog Notice that the table shows the elements in a column labeled Component It is in this column that you enter the stoichiometry For example if you wish to calculate Mn as an oxide change the text in the column for Mn from Mn to MnO2 Each of the elements in the table can be changed to oxides if desired As another example Fe could be entered as Fe203 Some components must be entered with a space between single character elements in order to avoid ambiguity An example of this is CaC O3 In this case if a space had not been used between C and O it would have been assumed to be Co cobalt Care should be taken in entering components to avoid such ambiguous entries In the above examples of components if O was not already on the element list it would have been added automatically Please check to
111. map after acquisition A Stitched Maps5 mpfs tlp els a aX Ofset 3 Yorset O Note prior to editing or exporting a stitched image map it is highly recommended that you save the stitched image map Tick marks on the perimeter of the maps indicate the boundaries of the 4 maps t ties The toolbar buttons can be used to manually slide the images left right and up down to align the data fields To align a field first click on it to select it A red cursor will appear as shown in the example above 134 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 Once a field is selected use the arrow buttons on the toolbar to adjust the position of the field The offset in pixels is given for the selected field In the example above the selected field has been moved 3 pixels to the right and no vertical adjustment 0 Multiple fields can be selected to move a group of fields together To select multiple fields hold the Shift key on the keyboard and click on the fields The buttons on the toolbar can be used to zoom in on the fields This is useful for fine adjustment of the field offsets 12 3 Saving and Exporting Stitched Image Map files are saved in a format different from images and maps in that they contain a collection of images maps It is important to save the stitched images maps after acquisition and also after any editing has been performed in order to retain the data Select File Save As from the menu
112. n This will include the energy range cursor marker etc e Customize Rendering Selecting this option allows for setting the energy range for the spectrum and other customizations described below The rendering options can be selectively applied to Printing Exporting and Clipboard output The selection is done in the Apply To section of this panel The spectrum rendering customizations are e Set Range to Enter the energy range that you desire for the spectrum rendering e Hide Cursor The vertical cursor can be useful during qualitative analysis of the spectrum but may be a distraction in the rendered output This option allows hiding of the cursor in the rendered spectrum e Auto Vertical Scale Select this option to have the spectrum scaled automatically during rendering e Restore Raw Spectrum After quantitation the spectrum displayed is normally the processed e g background removed spectrum It is common to want to output the raw spectrum non processed in reports This option will automatically render the raw spectrum e Clear Spectrum Overlay After quantitation an overlay of the fitted peaks is typically displayed Select this option to remove the overlay from the rendered spectrum e Hide MLK Buttons The MLK buttons below the spectrum are useful for peak identification but are not necessary for printed reports Selecting this option will hide these buttons 4 9 Exporting Files Spectrum data files can be exported
113. n either the Mn K 5 772 6 026 Always Present color or the Automatic Identification color e E 6 273 6 535 Elements can be added and removed from the x ray linescan 0 795 7 065 element list via selection on this periodic chart Ni 1 339 7 617 Scale Linescans selects the method of display for the linescans Li B Note If the x ray linescan has been loaded from a disk file Set As Defaut Save Settings Load Settings and the spectra data have not been stored in the file it will not be possible to produce linescans for new elements 125 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 The Element Settings section of this panel is used to further refine the element list The integration region ROI for each element can be adjusted Note that a unique color is displayed to the right of each element in the list This color corresponds to the colored regions of the spectrum displayed below the linescans After changing the ROI for an element it is necessary to press the Update Graphs button to apply the changes made The element linescans are constructed using the x rays whose energy are close to the selected line e g Ka La Ma Default lines are selected for each element when the element is added to the element list Clicking in the Line column of the table modifies the line selected for each element When making a new selection for line the Low keV and High keV entries in the table are updated The Low keV and Hig
114. n selected a materials class can be selected from the database A single database can store many materials classes A materials class is a set of material specifications These specifications will be used to classify each sample analysis Below are the steps to setting up Materials Classification 80 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 Enable Materials Classification Select or Create a Database Select or Create a Materials Class Edit Materials in the Materials Class Test the Materials Class with samples 4 16 1 Enable Materials Classification To begin using Material Classification it must first be enabled in the spectrum Properties Quantitation tab Click on the Materials Classification button and a panel similar to the following will appear a JE terial Classific ation l ea Click the Enable checkbox as shown above 81 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 4 16 2 Select or Create a Database The Material Classification material specifications is stored in an input database file This is a Microsoft Access database file that contains specific tables designed for storage of the Material Classification data When the software is installed an empty input database named input mdb is created This can be used or a new database can be created To select an existing database file click on the Browse button To create a new database file click on the New
115. nel Types Solid Grid Flat Components Border Axis Side Legend Base ma 3D Color iq Zoom The 3D control panel sets up the basic display type for the 3D view Types of view are Solid as shown above Grid or Flat Grid type displays the image with a mesh of lines Flat type is identical to the normal image presentation with no height Z information The image can have Border Sides Base Axis and Legends added by selecting them from this control panel The legend is useful in correlating the color to a Z height 117 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 9 17 2 Color Control Panel Back Color CL v Border Color C Gradient Custom Gradient color Division 10 Custom color Division 10 5 The Color control panel establishes the colors used for the image Back Color sets the background color for display Border Color sets the border and axis label colors Gradient color defines the colors used for the image by setting a color for the Minimum and Maximum heights and a Division for gradient A palette of colors for the image is then automatically generated Custom Color allows for setting up custom colors for each Division 118 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 9 17 3 Zoom Control Panel Move Fotation O Move Rotate Render Fast Auto Render Fast Full Render 512 The Zoom Control pa
116. nel allows for zoom rotation and moving of the image The Zoom slider adjusts the size of the image The Move or Rotate options select the mouse actions When Move is selected dragging the mouse over the image will slide the image in the direction of the dragging When Rotate or Center Rotate are selected dragging the mouse will rotate the image The Render Fast option displays the 3D image in a reduced resolution This can be useful for large images when rotating or moving the image is slow With the Auto Render Fast option enabled anytime the mouse is used to rotate or move the image the image is automatically rendered in fast mode reduced resolution Full Render is the maximum resolution that the image will be displayed at when not in Render Fast mode The Full Render resolution maximum resolution is 1024 or the original data resolution whichever is smaller 9 17 4 3D Menu File Print File Print Preview File Print Setup These are standard printing options Edit Copy Copies the 3D view to the windows clipboard 9 18 X ray Map Drift Correction 119 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 Some samples are difficult to acquire x ray maps from because of sample drift during acquisition of the map Quality x ray maps may take more than 2 hour of acquisition time During this time certain samples may drift horizontally or vertically This drift will cause a blurring of the maps It is possible to det
117. nel similar to the following will appear to allow for selection of a line for the linescan on the image A horizontal line can be selected on the image with the button An arbitrary line on the image can be selected with the button After selecting a line on the image with one of the above tools the linescan is automatically acquired You may stop acquisition of the linescan and adjust the linescan acquisition parameters if desired Note in the EDS application the image in the linescan window has a menu identical to a digital image menu Be sure to click over the linescan not the image to access the linescan menu items 10 2 Setting Acquisition Properties The x ray linescan acquisition properties should be optimized for the specific sample To access the acquisition properties select Properties from the x ray linescan menu The acquisition properties are found on the Acquisition tab of the x ray linescan properties panel Resolution 128 Default Xray Linescan Properties in Acquistion Element Selection Quantitation _ Point Dwell 50 000 mSec Sec Point Dwell is the acquire time per point The time is given Multi Scan Max Scans in either milliseconds mSec or microseconds uSec Use Taer a SL microseconds when specifying short dwell times e g below 1 mSec Increasing the Point Dwell time will generally improve the quality of x ray linescan as larger iit a number of x
118. nt ROIs for maps and linescans is 1 8 FWHM around the peak center To the left is an example of the ROI for Fe using one FWHM By setting the ROI Width to 2 0 most of the peak area is included in the map for Fe as shown below Restore Default ROI will return ROI Width to its factory setting Setup Palettes allows for configuration of the default palettes SEM Palette allows for changing of the display color of the SEM image If the ROI is changed for an element the Update Graphs button is enabled Clicking on this button will recalculate the maps using the new ROIs integration regions The Element Settings table displays settings for each element including color ROI integration region and display settings Below is a description of the table settings T a Map Color Click on the color block to the left of an element to change the map color Line The line for the element map can be selected The default ROI integration region will be selected updating the Low keV and High keV settings Note that the ROI Width is used to determine the default ROI Low keV High keV The integration range for the element maps can be customized by changing these values Threshold This column displays the intensity threshold for each element In the example above carbon has a threshold of 4 49 counts Clicking on the Threshold column for an element displays the histogram from the element See the section View Histogram on page 102 for d
119. ntane nateiet ie A 49 4 10 9 Sclection of Blement Analysis Lines accion cise a N 49 AOJO Gamar DECOny NON e E a RN 32 Als WWCteCLOR L OME e a drama a tceen aes 54 4 11 1 One ANos DECECO 5 CEU oie tedsg ti laia a aa a a a tees 55 4 11 2 ORAS Detector GEomMme Ierse a T a a a 56 ANZ Detector SCIP eere a a E a E eE E 57 4 12 1 Window Parameters gi acconacecsetescececamsscncistsdnceeacasceceus ecebetmaseucecncecseemsceede E ENE 57 4122 Detector Para metot cenen aE a aa Caen VE T T E A 58 4 13 ZAF Quantitative Analysis using Standards ccccccccccccceccececeeasseessseseeeceeeeeeeeeeeeeseeeaaaeseeees 59 4 13 1 Standardless VS Standards scacccesiscchseasdicckcscPacoreacacds es E EA O E E 59 4 13 2 CIO EAU OINS sana a a cesian ot ese ae tnd aetna tacsndanentuatiuesek 60 4 13 3 Creatinged ZAR alibramOm Piesa ctaudenmaeiceuontedaumeauan 60 4 13 4 Performing ZAF Quantitation with Standards ccccccsssssssssssseeeeeceeeceeeeeeaaaeaeseseeeeeeeeeess 64 4 13 5 ZAF NV ATT sand EMOS epeen e e len adtaebsadeudedsanmatoneatagqusennantundadeoanean 65 AA Mark AIAN SIS e a a N 66 4 14 1 Q alhiaive Mate rANAlVS IS sopi a a a 67 4 14 2 Oirantitative MateMAnalySiS ccrois aeea Eee E EEEE 69 4 14 3 Wie w 1 VIALCIb RR CSUMS i s sassusssccondsncomautnse cagsaaneehsansedsnenunawinaeiusatesmnusebenooadmeomatnansenccmiuncls 70 AVS iLedst Squares Quantitation methodos dea couns EEEE EE 71 4 15 1 Creatine the calibra on Teepee a means tensinascunces
120. ntense OQ Thermal A color palette based upon a thermal color scale is constructed QO RGB A color palette is constructed which spans the Red Green and Blue ranges specified The ranges are given as numbers between O least bright to 255 most bright 98 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 9 3 1 1 Pseudo Gray Color Palettes To create a Pseudo Gray color palette click on the Pseudo Gray button The following Windows color selection dialog will appear Color Basic colors Select a color This will be the base color for the palette In this fa T LET fae example an orange color has been selected The color palette will be inn ion constructed such that the least intense areas of the map will be black As toes fon 0 5 mn T the map E E es a mea me Hi E TAT ase co or will appear e most intense areas of the map will be white Below is an example of the orange color palette created from the EEE eee selection to the left EES E Custom colors BEE Een ee ep pe ee NE Define Custom Colors gt gt cance 9 3 1 2 Thermal Color Palette To create a thermal palette click on the Thermal button The following palette will be constructed and displayed in the dialog 9 3 1 3 RGB Color Palette RGB Red 259 0 To create a RGB color palette first select ranges of Red Green and Blue for the palette Next click on the Set button Shown here are ranges for an inverted red p
121. ntitative analysis the elements that are to be quantified must be specified in the element list for the spectrum Automatic and manual peak identification methods are provided Manual peak identification can be done using any of these tools e Element ID Buttons e Periodic Table e Cursor Identification 4 7 1 Element ID Buttons Element ID Buttons are displayed below the Energy Scale on a spectrum These buttons are located at the position of the Ka peak for each element Clicking on these buttons will add the element to the list of identified elements in the spectrum and display the MLK markers for the element At certain display resolutions there may be a bar at the upper left corner of the element ID buttons in the same color chosen for the markers This indicates the position of the K line 32 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 4 7 2 Periodic Table A Periodic table can be displayed from the View Period Table menu item or from the ToolBar button a To add elements Cu Zn Ga Ge As Se Br manually to the element list select Always d Ag Cd In Sn Sb Te I Xel aa Au Hg TI Pb Bi Po At Re the buttons on the periodic chart to display at the bottom of the panel and then click on the MLK markers for any element Using u Gd Tb Dy Ho Er Tm Yb Lu the P
122. nu A panel similar to the following will appear This panel is identical in function to the Element Quantitative x ray maps above ox Create Quantitative Component Map Sase v Quantify Using OY Display Processing Whole Spectra Start lt Use Quick Linear Gauss 9 12 Viewing Quantitative Maps To select viewing of the Intensities Quantitative Element or Quantitative Component maps use the View menu as shown below Acquire OONO O Clear File Edit b Intensities Concentrations Process Overlay Elements Composition Properties gt Create Linescan From Map w Intensity Maps Quantitative Element Maps Quantitative Component Maps Info w All Spectral Data Drift Gorrection History 110 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 9 13 Quantifying X ray Maps Composition Composition analysis of x ray maps is designed to find locations on a map that contain specified elemental concentrations Quantification is performed on each pixel point in the map and the calculated elemental concentrations are compared to the specified concentrations The pixels that match the specification are then displayed in a separate map To perform the composition analysis select View Composition from the menu The following panel will appear Below is the new X ray Map Composition Tool panel TE X Map Compe Element Concentrations Composition Descrip
123. o transparent maps no maps visible Note If the x ray map has been loaded from a disk file and the spectra data have not been stored in the file it will not be possible to produce maps for new elements Adjusting Color Palettes for X ray Maps The color palettes for each element and the SEM image can be adjusted Adjustments in the contrast and brightness of maps can reveal subtle details in the maps that are not visible with the default settings Each element and the SEM image have a separate color palette contrast and brightness settings Elt Line Bc k amp The color palettes for elements are adjusted in the Element Selection tab of the Properties panel To adjust the color palette click on the button to the left of the element symbol as shown above for carbon The following panel will be displayed Adjusting the contrast and brightness can reveal hidden detail in the maps Increasing contrast will tend to reveal small variations in the x ray map Areas that appear to Thema be of the same intensity but actually have small variations Load File will be more visible Increases of contrast may require a Save File decrease in brightness so as not to saturate the x ray map Spectrum Window Color Color palettes can be created by a err O Pseudo Gray A color palette is created from a base color The palette spans through the base color from a starting color of black least intense through white most i
124. ocation of the previously acquired data select View Go To Stage Location This will move the stage to the location where the data were acquired 9 3 Setting Element Properties The element list used for the x ray map is the current element list from the last EDS acquisition For example if a spectrum was acquired and peaks were labeled either manually or using automatic peak identification the labeled elements will be the element list for the next x ray map acquired Further refinement of this list can be done with the Element Selection tab of the X ray Map Properties To access the x ray map properties select Properties from the x ray map menu Above is the Element Selection tab The elements that will be mapped are indicated on the periodic chart in either the Always Present color or the Automatic Identification color Elements can be added and removed from the x ray map element list via selection on this periodic chart 96 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 When the Enable Quick Select option is enabled elements can be added or removed from the map with the manual element ID features of the Sum Spectrum or the Maximum Pixel Spectrum These tools include the Element labels on the horizontal axis of the spectrum as well as the Periodic Chart tool for the spectrum Remove All clears the element list ROI Width is used to calculate the default ROI integration region for elements By default the eleme
125. odic chart The elements are color coded The color coding is described in the Periodic Chart dialog Elements in this list are considered to never be present in a spectrum This list is useful for automatic element identification in that it helps to restrict the possibilities for identification of elements in each peak All elements that are known to never be in a spectrum should be added to this list to improve the reliability of the Auto ID Print Coxe 4 8 Customizing Spectrum Rendering for ae Printer System Printer HP Photosmart C7200 Printing Exporting and Clipboard OE ee en Print Range Cancel Spectrum rendering can be customized using the Tee Spectrum Options setup Access to the Spectrum Sdlaction Options setup is available on the spectrum Print r panel as shown below and also on the Export and To To Export to Word panels Print Quality 600 dpi Copies Print to File Print i Spectrum C Spectrum Options y i Quantitative Analysis Image 36 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 Clicking the Spectrum Options button displays a panel similar to the following Spectrum Rendering Options 0 000 10 000 clic user O Resoc pay specin Ant Veiga scade Wes speci Uvrenay There are two primary settings for the spectrum rendering e Render Exactly as Displayed The rendering will render the spectrum as closely as possible to what is displayed on the scree
126. on Settings option This will copy the calibration settings for the selected Time Constant to all of the other Time Constants thus setting up all of the other Time Constants to reasonable settings Click on the Copy Calibration Settings button and a dialog similar to the one here will appear Click on OK to copy these settings to all other Time Constants __ ___ _ If you have performed the Copy Calibration Settings it is recommended to acquire a spectrum at each of the remaining Time Constants to ensure that the settings for Gain Threshold and Slow Threshold are reasonable Select another Time Constant from the Energy Calibration panel and acquire a spectrum If the peak positions are more than 100 eV from their correct locations a small adjustment of the Fine Gain may be necessary Also if a noise peak appears at the low energy region of the spectrum a slight adjustment of the Slow Threshold and or Threshold will be required If you have not performed the Copy Calibration Settings repeat steps through 8 for each of the remaining Time Constants When all Time Constants have been calibrated proceed to the Automatic Energy Calibration Note If it is impossible to remove the noise peak using the Thresholds as described above it may be necessary to disable the Base Threshold AutoSet and adjust it manually To manually adjust the Base Threshold do the following 1 Unselect AutoSet option 2 Increase Base Threshold until t
127. on and select the standard file Once the standard file has been selected you can use the View button to examine and modify the file as desired 62 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 Click on the Calibrate button to perform the ZAF calibration When the calibration is complete a dialog similar to this will appear Save As 2 x Save in a EDS Data E ff e E save as lype ZAF Cal Files fpc Cancel The dialog shown below will appear fi dium Ultra Merge this calibration with Existing file calibration Enter a name for the ZAF calibration file and click the Save button to write the coefficient file with fpc extension to disk The ZAF Calibration is now completed This procedure can be repeated for other standards and the coefficients can be stored in separate calibration files one for each standard or merged into a single calibration file If you choose to merge the calibration coefficients into a single file begin by selecting an existing calibration file for storing the calibration coefficients Selecting Yes will confirm that you wish to merge the present calibration into an existing calibration file Selecting No will proceed to replace the existing calibration file with the present ee If you are merging calibrations and there are any elements in the present calibration that are also in the existing calibration file a dialog will be pres
128. on the Start button This will begin acquiring spectra After the acquisition of each spectrum the FWHM peak center FWThM and FWThM FWHM will be calculated and displayed in the panel Statistical calculations of Minimum Maximum Mean and Standard Deviation STD will be calculated 6 At the end of the calculation the Mean value for the FWHM can be used for the FWHM of the current time constant Click on the Update System FWHM button to store this value permanently This FWHM will be used for processing of all spectra acquired with this time constant Note that spectra acquired before this action will use the previous stored value for FWHM 7 You may wish to print and or copy the results of the FWHM calculation 8 Repeat this procedure for each time constant Calculate At Cursor This calculates the FWHM at the cursor location on the spectrum It can be used to measure the FWHM of any peak without the need to acquire the spectrum This can be useful for previously acquired spectra and also for measuring FWHM of peaks other than Mn Calculation Method There are two methods for calculating FWHM Curve Fit uses a theoretical gaussian model fit to the spectrum The FWHM is calculated from this theoretical fit Because Curve Fit uses a theoretical model of the spectrum the FWThM is set to the FWHM Interpolation finds the half maximum data channels above and below the peak center channel Interpolation is the technique used to find mi
129. ondensation of any water vapor present in the system Sometimes this water vapor comes from the detector cryostat itself as it starts to outgas if there is a materials problem In any case a significant ice coating is usually a sign that the detector is in need of repair If the ice is observed on the outside of the detector housing and or window then this almost certainly means that a detector repair is necessary An estimate of the ice thickness can be entered in nanometers as a method for compensating for the absorption of x rays by the ice layer to improve the accuracy of standardless analysis 4 13 ZAF Quantitative Analysis using Standards 4 13 1 Standardless vs Standards ZAF quantitative analysis can be used with or without standards The primary reason for using standards is to improve the accuracy of the composition analysis of the sample Standardless analysis can achieve typical errors in concentration of less than 10 relative but they can be as high as 50 When calibrating with standards errors of less than 5 relative are typical There will be occasions especially when mixing lines from different series e g K and L where much improvement can be made in the analysis by using standards The downside to calibrating with standards is that the beam current should ideally be maintained at a constant level for all standards and unknowns something that is easy to achieve with many SEMs If results are normalized to 100 then t
130. ons on the sample that you wish to analyze As the locations are selected they will be labeled on the sample and entered into the list in the panel as shown below faa Cear us Delte Po Selected Positions Add Labe Hame A YT Imagel 1 665 419 Tagel 419 998 Imagel 3 439 1 684 5 2 Adding Labeled Locations On systems that have automatic particle analysis the Add Labeled button will appear Clicking this button will add all of the automatically located particles to the list 85 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 5 3 Selecting Analysis Settings es Acquisition and Analysis Settings The spectra will be acquired and analyzing using either the present default Use Present Settings settings or a selected settings file The selection is displayed in the Acquisition and Analysis Settings section of the panel as shown at right tin ti iT Use Present Settings In this example the present selection is to Use Present Settings To select a settings file click on the Select Settings File button and select the settings file that you wish to use Below is an example of using a selected settings file e microdat oxides def Acquisition and Analysis Settings Use Present Settings 5 4 Selecting Location for File Storage The spectra data acquired are stored in the location selected here To select a different folder for storage click on the Br
131. onstant used for x ray mapping For example for a Point Dwell time of 50 uSec the largest Time Constant that should be used is 12 5 50 4 The reason for this is ensure that the x rays acquired for each point are actually from that beam position A finite amount of time is required to process an x ray through the electronics This time is related to the Time Constant Larger values of Time Constant require more time to process each x ray The Estimated Acquire Time is the amount of time to acquire 1 frame number of pixels in X times number of pixels in Y times dwell time pixel If Multi Scan is enabled then the total time to acquire the map is the estimated acquire time frame x the number of scans frames All calculated times are approximate Resolution is the number of pixels across the longest side EEE I Of the rectangular area of the x ray map If the area of the X ray map is a square Resolution applies to both the vertical and horizontal sides of the rectangle Larger values for Resolution will require more time for acquisition but will also yield greater spatial resolution For example a 256 resolution square x ray map with a pixel dwell time of 50 mSec will take approximately one hour to complete a scan If the Resolution is reduced to 128 it will take approximately 14 minutes The selection of Resolution should be made large enough such that the features that are being observed can be seen clearly and their positions accurately def
132. or and the counts number of x rays in the channel In addition a Cursor ID List is displayed which identifies the closest matching x ray lines near the Cursor Position Element ID Buttons are displayed below the Energy Scale These buttons are located at the position of the Ka peak for each element Note there is a small bar in the same color as that chosen for the markers at the upper left corner of the buttons This indicates the position of the K line for each element Clicking on these buttons will add the element to the list of identified elements in the spectrum and display the MLK 25 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 markers for the element Itis also possible to add elements by double clicking on an element on the Cursor ID List The Vertical Scale of the spectrum is displayed below the Cursor Position To the right of this is the Spectrum Integral The Spectrum integral normally shows the whole spectrum integral typically 0 40 keV It can optionally display a specific energy integral using the d ToolBar button 4 1 Acquiring Spectra Click on one of the Spectrum Acquisition buttons on the EDS ToolBar This will create a new Spectrum window and start acquisition of the spectrum Ie ne EOI OCCT ID tel SEN ROMO WANE CULE ICI Rte ene INSEE Start Clear Resume Start If the spectrum is not presently acquiring this continues the spectrum acquisition If the spectrum is acquiring a
133. or maximum This will result in any possible value of concentration for that element to be acceptable Note that when an element is added to the material it is added to all materials and that the initial range setting is O to 0 A range of 0 to 0 indicates that the element is absent from the material This may present problems in classifications Using ZAF or any quantitative analysis method there is always a possibility of a small concentration of an element detected even though the element is not present in the sample This could be caused by incomplete background removal or in the peak deconvolution process It is best to have a small value for the maximum for all elements even though the elements may not be present in the sample Click on the Add Material button to add a new material to the Materials Classification A prompt will appear to enter the name for the new material Clicking the Delete Material button removes the selected material from the Materials Classification To add an element click on the Add Element button A dialog is presented for entry of the new element symbol Note that after entering a new element to the materials specification that the range of concentrations for all materials in this Materials Class must be entered To delete an element click on the Delete Element button This removes an element from all materials in the Materials Classification Properties ARF Calibration Std 1 4 16 5 Test the Materials Class wit
134. overlays etc 136 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 14 Energy Calibration Energy Calibration and related setup and calibration of our Models 500 5501 Digital Pulse Processor DPP are accessed from the Utility Energy Calibration menu item of a spectrum When performing any of these operations it will first be necessary to have a spectrum Refer the section on Working With Spectra if you are unfamiliar with acquiring spectra Selecting Utility Energy Calibration from the menu will display a panel similar to the following Automatic Manual Advanced FWHM Low Energy Calibration 14 1 Offset DAC Calibration Model 500 only Whenever a detector is connected to our Model 500 Digital Pulse Processor DPP for the first time the Offset DAC Calibration must be performed This is only necessary with revisions A and B and C of the Model 510 To determine the revision of the DPP click on the Advanced tab on the Energy Calibration panel as shown below In the above example the revision is D the Calibrate Offset DAC is not necessary To perform the Offset DAC Calibration do the following 1 The power on the DPP should be turned on for at least one hour prior to performing this calibration If the power is off turn on the power and continue with this calibration after one hour 2 With the Energy Calibration displayed click on the Advanced tab A panel similar to the one shown above will ap
135. ow energy peaks should now appear in the correct position in the spectrum and the higher energy peaks should also remain in their proper calibrated locations This low energy calibration should be performed for each of the time constants that you expect to use You should not have to perform this calibration each time you do a normal energy calibration This calibration should normally be required only once 142 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 14 5 View Input As an aid in trouble shooting the Input signal can be viewed Automatic Manual Advanced FWHM Low Energy Calibration This is accessed from the Advanced tab of the Energy Calibration panel as shown _ View Baseline Fimware Revision 0 00 FIPPI Revision A View Input Trace Enable Baseline Cut 10 Default Calibrate Offset DAC Digital Pulse Processor Revision D Diagnostics Inhibit Time 1 psec Default Click on View Input Trace A View DPP Spectrum dialog similar to below will appear ae Pulse Processor Input Trace This is an example of Mn X rays Each vertical step is proportional to the energy of the event The downward slope is caused by a ramp signal which has been added to the input to keep it within the ADC input range The Sample Period can be changed to view 550 450 longer or shorter time periods 400 The Sample Period entered in microseconds is the time between 350 e
136. owse button Save Spectra In Directory CAXRFDATA Browse 5 5 Selecting Report Output Options Upon completion of the acquisition and analysis of the spectra printed output and a Spectrum Report summarizing the elemental composition of all of the spectra can be generated Below are the options for output Generate Spectrum Report Print Options Reports Auto ID Spectra Generate Spectrum Report tabulates the elemental composition from the spectra and calculates statistics on the elemental analysis mean minimum maximum standard deviation This report can then be printed or copied into another application Printed output can be any of the following Q Reports This is the quantitative analysis report as specified in the analysis settings This may include component and or elemental analysis Q Auto ID Prints the output of the automatic peak identification on the spectrum QO Spectra Prints the spectrum 5 6 Starting the Analysis Click on the Acquire button to begin the automatic acquisition and analysis of the locations on the sample The Start button will be replaced with a Stop button Click on this button to terminate the process During acquisition the spectrum data is displayed at the bottom of this panel Note the application Acquire button does not stop the acquisition use the Stop button in this panel to terminate the acquisition 5 7 Saving and Loading Location Files If you wish to use the same location
137. pear Click on the Calibrate Offset DAC button 3 A dialog similar to the following will appear Click on the Calibrate button 137 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 OK Cancel Oltset 234 Manual Cal gt gt Manual Cal lt lt 4 After a few seconds a histogram will appear It should be centered which indicates that the signal falls within the range of the input of the DPP 5 Click OK 6 The Offset DAC Calibration is now completed 14 2 Manual Energy Calibration and Threshold Adjustments Default Spectrum Properties ES Whenever a detector is connected to our Models 500 5501 AY Acisi Blement ID Digital Pulse Processor DPP for the first time Manual Energy Calibration and Threshold Adjustments are required Manual Energy Calibration adjusts the gain and zero settings of the DPP such that the peaks in the spectrum are in approximately the correct locations This is necessary before performing Threshold Adjustments After performing Manual Energy Calibration and Threshold Adjustments the Automatic Energy Calibration should be performed This will ensure that the DPP 1s finely calibrated There should be a known sample with two well separated peaks such as Al and Cu in the microscope The power on the DPP should be turned on for at least one hour prior to performing this calibration If the power is off turn on the power and continue with this calibration after
138. pecification defining the allowed range of the elemental compositions This is a partial description of the elemental composition of the three materials Only the concentrations for Fe and Cr are given Each of the concentrations is given as an acceptable range minimum and maximum When a sample is classified after being quantified its concentrations are compared against the Materials Specifications in the selected Materials Classification If the element concentrations are within the range of acceptable values for a Material Specification then it is considered to be matching that material After this classification process the sample may have zero or more matches with materials in the Materials Classification The name of the best matching material based upon computed chi square fit 1s stored in the Output Database To begin setting up the Materials Classification select the Material Classification properties from the Spectrum Properties panel as shown below To access the Spectrum Properties select Properties from any spectrum s menu or from the menu on the EDS Toolbar The Material Classification properties define the set of materials from which the classification of the spectrum will be made The Material Classification are stored in a Microsoft Access database file The first step in defining the Material Classification is to select a database file If no database files exist a new database file can be created Once a database file has bee
139. pectrum that will be used for normalization during the spectrum comparison The default is the whole spectrum 0 0 kV e Fit Region This defines the region of the spectrum that will be used for comparison The default region ROD is the whole spectrum 0 0 kV In some cases only a selected region of the spectrum should be used for comparison excluding all other channels For example if match is to consider only the fitting of the peaks for Cr Mn Fe and Ni a ROI of 5 0 9 0 kV would be appropriate This would indicate that any peaks above or below this ROI would not be considered in the comparison 4 14 2 Quantitative Match Analysis To setup an analysis using quantitative match the following need to be done e Proceed as per the Qualitative Match analysis E i see above and then create a standard file Component Conc Units for each of the above spectra To create a 3 Lal4 wi standard file select Utility Create Standard Cr 20 983 wh from the menu A dialog similar to the Mn L815 ws following will appear ve The Component concentrations are those from any analysis that has been previously done on the ancentration Total 100 00 wi spectrum Components can be added to the standard P using the Add Component button A new row will O K appear in the Component table Enter the Component i zone sai Cancel e g Fe203 Components can be removed from the aes Save table by selecting them with the mouse
140. ponent Table above The Quantitation Display settings are stored in settings files just as the Quantitation settings are stored At this time you may wish to save these settings for use in the future Use the Save Settings option of the spectrum Properties to store these settings 4 10 6 Using the Manual Processing Tool The Manual Processing Tool allows the user to step through the spectrum processing viewing the effects of each step on the spectrum To access the tool select Utility Manual Processing from the menu A dialog similar the following will appear ian Remove Escape Peaks m Remove Sum Peaks Remove Background Deconvolute 46 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 Each of the spectrum processing steps is assigned to a button on the left side of the dialog To step through the spectrum processing click on the buttons as they are enabled Only buttons that are enabled not grayed out are active In the example shown below only Smooth Restore Spectrum and Estimate kV are enabled All other buttons are disabled Clicking on the Smooth button will perform that step and display the modified spectrum After clicking on the Smooth button the next processing button will be enabled and the Smooth button will be disabled In most cases this will be the Remove Escape Peaks button Only the steps that have been selected on the Quantitation tab of the Spectrum Properties will be allowed For exampl
141. ppear Fast LineS can Spectrum Report Least Squares Calibration Stages can Stage Map Stitched Images Stitched Maps VP Mode Spectrum Select VP Mode Spectrum A panel similar to the following will appear a TVP Mode Spectrum ee YP Analysis Elt Line Intensty Error Conc cls 2 sig 0 000 wtTotal kW 0 0 Takeo Angle 28 6 Elapsed Livetime 1 5 Variable Pressure Settings VP 0 000 mbar VEZ 0 000 mbar Air For VP quantitation two spectra must be acquired at different pressures In this panel the two spectra are labeled VPI and VP2 To acquire the spectra do the following 92 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 1 Select an appropriate pressure on the SEM for the sample 2 Right click over the VP1 spectrum and from the menu select Properties A panel similar to the following will appear Enter the VP Mode information pressure units and Atmosphere O a ohal i Acquisition 3 Click on the Acquire button to start spectrum acquisition A panel similar to the following will appear Select the Acquire spectrum VPI or VP2 4 Repeat steps 1 3 for the VP2 spectrum 8 3 Quantifying VP Spectra Quantitation is done by selecting ZAF as the quantitation method The two spectra will be automatically processed No other quantitation methods are presently supported with VP Spectra 93 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 9 Working
142. pplication Warning The following element calibrations are gt 5kV from this spectrum A list of elements will follow on the next line on the screen The elements listed were calibrated at a kV significantly different from the present spectrum The calibration file may not be appropriate for this analysis Warning The following element calibrations are for different lines than this spectrum A list of elements will follow on the next line on the screen The elements listed were calibrated with a different analysis line e g Ka instead of La than that of the calibration file Warning No Calibration File for Cr Fe A list of elements shown Cr and Fe in this example is displayed of all the elements that do not have a calibration file specified These elements will use an interpolated calibration value derived from the calibrated elements values Warning Elements not in specified Calibration File Cr Fe A list of elements shown as Cr and Fe in this example is displayed of elements which are not in the calibration file specified In this example a calibration file was specified for both Cr and Fe but the calibration file does not have these elements 4 14 Match Analysis Match can be used to perform Quantitative or Qualitative analysis When used for qualitative analysis the spectrum being analyzed is compared with spectra stored on disk The best matching spectra using a chi Square criteria are displayed When used for qu
143. primary ionization effects and detector absorption factors are specifically eliminated The user should be aware that these values are still used in the software for ZAF analysis so one should not change them between calibration and quantitation The reason this is done is so that missing elements can be analyzed by estimating their calibration coefficients from both adjacent elements in the periodic table and from the use of these fundamental parameters Because many of these primary effects have some uncertainty either from the basic physics knowledge or lack of knowledge about the experimental setup e g detector parameters the use of standards can eliminate many of these sources of error Most ZAF techniques use pure element standards where the first step in the calculations involves the calculation of the k ratio 1 e the ratio of the element s intensity in the sample to that in the pure element standard This automatically removes many of the calculations used for standardless analysis However in the software the calculations are done differently so that any standard can be used If available there are many advantages in using a standard that is similar to the unknown sample If all the elements are the same a single type standard can be used to calibrate the system In addition to compensating for the primary effects described previously these type standards can compensate for secondary inter element uncertaintie
144. r elements added to the element list In this table there are two methods that can be used to select the element line e Use kV This method determines the best line automatically from the kV of the spectrum The user has no choice for overriding the automatic selection To use this method select the Use kV check box Automatic line selection uses the kV of the microscope The line selected is the line whose absorption edge is below the kV e From the Table This method takes the line from the table shown on the left side of the dialog above To use this method unselect Use kV When using the Table method you can select the lines individually for each element If for example you wish to use the Moa line for W analysis instead of the default which is La do the following ise Line Energy 146 3 398 Find W in the Table Select Ma from the list of lines 50 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 The second method to select the line for analysis works on an individual spectrum or for a specific Settings File This method uses the Advanced dialog on the Quantitation tab of the Spectrum Properties as shown here Click on the Advanced button in the Quantitation section and a dialog similar to the following will appear Select a line from the list of lines for the element in the following example Cr in the lower of the two tables O cr a et by selecting Save Settings on the Spec
145. ratio will be allowed to vary from 0 5 2 0 25 up to 0 5 2 1 1 e same height as the parent Kal Spectrum Zero The positions of the peaks are allowed to shift in order to improve the fit This is the maximum shift in eV that is allowed Spectrum Gain The gain eV channel of the spectrum is allowed to change in order to improve the fit This is the percent of change that is allowed Spectrum Peak Width 53 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 The width of each peak is allowed to change in order to improve the fit This is the percent of change that is allowed As an example if the Mn Ka FWHM is 150 eV and the Spectrum Peak Width maximum deviation is 50 the width would be allowed to vary from 0 5 150 75 to 1 5 150 225 eV for Mn Ka 4 11 Detector Geometry The geometry of the EDS detector is critical information required for ZAF quantitation It is important to have the correct information entered in the system in order to get good quantitation analysis The set of geometry parameters describe the spatial relationship of the EDS detector with respect to the electron beam and the sample To setup the detector geometry click on the Geometry Setup button on the spectrum Quantitation panel as shown below For many detectors there is a very simple set of parameters required for describing the geometry These detectors are known as on axis detectors An on axis detector is one in which t
146. ration Std 2 um Properties dialog as shown below m E Fill in the Match Setup as described below e Save the Analysis Settings so that they can be used on future spectra acquired e Quantitative analysis of a spectrum using these settings will now perform qualitative Match analysis Match Setup As a minimum Match needs to know the location of the match spectra directories and whether to perform quantitative or qualitative analysis To specify this information and more click on the Match Setup button on the Quantitation tab of the Spectrum Properties dialog A dialog similar to the following will appear E microdat 6D ata One or more directories must be selected Click on the Add button to insert a directory into the list of selected directories To take a directory out of the list select it by clicking on it and then click the Remove button 68 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 Be sure that the setting for Quantify is set to your specific needs If you wish to produce quantitative analysis i e elemental composition you will need to select Quantify Of course this also will mean that you will need to create standard files for each spectrum you wish to match against For qualitative analysis Quantify should not be selected There are two regions of the spectrum that can be used to control the matching process e Normalization Region This defines the region of the s
147. re You can set everything up ahead of time and collect the data while the microscope is unattended and when data collection has finished the beam will be turned off automatically 131 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 12 Stitched Images and Stitched Maps Image and Map stitching allow for acquisition of images maps over a large area This is done by moving the stage automatically or manually to adjacent fields forming a grid of images maps from the data acquired at each field This grid of images maps can be stitched together into a single image map file 12 1 Acquisition To acquire a stitched image map select File New from the menu and then select Stitched Images or Stitched Maps as shown below Create Analysis Data Fast LineSican Spectrum Report Least Squares Calibration Stages can Stage Map Stitched Images VP Mode Spectrum A panel similar to the following will appear Orthoclase 5 rex z DECECE Prior to acquiring the stitched image map setup the microscope at the desired magnification for the stitched image map Click on the Acquire button to begin acquisition of the stitched images maps A panel similar to the following will appear 132 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 test Wese Prssant Satire Microscope Stage This panel is used to setup the acquisition Name This is the stitched image f
148. rifting process there is often a thin layer at the front of the detector crystal that is inactive This inactive or dead layer cannot generate the usual charge cloud from the absorption of an x ray and effectively acts as an x ray filter to incoming x rays as a result Again it is important to enter this dead layer thickness in microns as it can affect the quality of standardless analysis This value should be provided by the detector vendor and will vary depending upon the quality of the detector crystal manufacturing Often this layer may increase slightly with time years as the Li ions slowly drift away from the front surface of the crystal Contact Material This is the material specified as an element that is used for the front contact of the high voltage bias connection to the detector crystal Sometimes this material 1s proprietary to the detector manufacturer It used to be always a gold contact but sometimes other elements such as Ni are used nowadays Contact Thickness This is the thickness in nanometers of the front contact layer Ice Contamination As with the deposition of oil on some windows see above there is sometimes a buildup of ice on the front surface of the detector crystal This is particularly the case if the detector is used in the windowless mode not very common these days or there is a small pinhole leak in the window material Again the detector crystal is often the coldest surface available causing c
149. rom the combined graph by selecting from the Composite list and then clicking on the lt button Another way to remove an element is to double click it After removing the element the graph will be re displayed with the remaining elements in the Composite list 10 5 1 Intensities or Concentrations The combined graph can be displayed as intensities or concentrations This is selected using the buttons in the View section above the graph 10 5 2 Overlay On Image For the EDS software the linescan can be overlaid on the SEM image Click on the Overlay On Image button to copy the combined graph onto the image Below is an example of a graph overlaid on the image The graph is now an annotation on the image The graph can be moved sized and deleted using the Edit Annotations panel for the image The graph can be moved but will always retain its alignment to the location that the linescan was acquired Otherwise moving and sizing the graph is done identically to other annotations on images text lines etc 10 5 3 Export Print and Clipboard The combined graph can be exported to a graphics file TIFF BMP etc printed or copied to the Windows clipboard ZOO 10 6 Printing Linescans Linescans can be printed using several pre defined styles For EDS systems the image can be printed with the linescans There are two basic printing styles as shown in the panel below 10 6 1 Single Page Output Style For this style al
150. rsor 6 390 bel 5357 ot ID Fe kat Fe kal Sm b Double Click here to add Fe to the element list When added it will be displayed colored green The element can be removed from the element list by double clicking it again 4 7 5 Customizing Display of MLK markers Customizing the MLK markers is done from the Display tab of the Spectrum Properties panel Click on the Setup butt the Display tab as sh below i cea ti lel A Properties IXRF Calibration Std 2 il A panel similar to the following will appear a Custom MLK Setup Labels Markers Labels Markers FI Lal La Lh1 Lh Lh3 Lh4 Lh6 Acquisition Element ID Quantitation Display r Spectrum Display Display and Print Settings k Setup No Markers Lgl ae Lo2 AllLabels Lo3 Al Markers ut L222 2 2 2 2 2 22 2 8 L222 822 2 2 2 2 2 2 8 a oo 2 2 2 2 2 2 2 SS 8 2 222 2 2 2 2 Ss Ss lt Seale Markers ta Parent Peak Each element has K L M x ray line series that are unique in energy for each element For some elements these energies can be too low or too high to be in the spectrum The line energy may be too low to be detected or so high that they are either not excited by the electron beam or are too high for the range of the spectrum or both For those line series that are excited detected and displayed the pattern of lines in those series can be used to match to or identify the pe
151. rum Simulation allows you to generate a synthetic spectrum based upon a given sample composition and excitation conditions kV This is accessible from the spectrum menu Utility Simulate Spectrum A panel similar to the following will appear To simulate a spectrum 1 Fill in the concentrations for the Components The Components as with Standard files can be single elements or compounds e g Fe or Fe203 Add components by clicking on Add Component Remove components by first selecting them in the list and then clicking on Del Component If you want to simulate the spectrum from a previously stored standard file select Load Standard This will fill in the Components from the selected Standard file 2 Inthe area labeled Simulate In selecting Bars will replace the spectrum presently displayed with the simulated spectrum Selecting Overlay will simulate the spectrum in the overlay of the present spectrum Thus the simulated spectrum can be easily compared with the present spectrum 3 Click on Simulate Spectrum This generates the simulated spectrum Clicking on Print to print the contents of this panel 1514 wt 20 983 wt 1815 wt 75 688 wt 1514 wt 20 983 wt 1815 wt 75 688 wL Synthetic Spectrum options are useful for those systems operating in virtual mode primarily as demonstration systems Normally when the EDS software is operating in virtual mode a synthetic spectrum is generated whenever data
152. s acquire a spectrum over the area of the linescan As the spectrum is being acquired adjust the microscope to get the highest countrate reasonable for the sample This is important because the beam may be moved rapidly 123 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 from point to point during the x ray linescan acquisition High countrates will improve the quality of the x ray linescans If the deadtime increases above 40 select a shorter Time Constant X ray linescans are typically acquired with a shorter time constant than spectra 10 1 2 Creating and Acquiring the X ray linescan dad To start acquiring an x ray linescan click on the button on the Toolbar For integrated EDS systems select a line on the image for the x ray linescan This is done using the mouse A crosshair cursor will appear on the image Click the left mouse at the vertical location of the line that you wish to scan To cancel the selection of the scan line and the acquisition of the linescan click the right mouse button Once the selection has been made the x ray linescan will begin acquisition The element list used for the x ray linescan is the default element list The default element list can be set from the toolbar properties of any of the EDS buttons spectra x ray maps linescans For EDS software the linescan will immediately start acquisition of a digital image to be used for the linescan After the image is acquired a pa
153. s as well as minor systematic errors in spectrum processing e g background removal and peak deconvolution In addition to the normal modes of calibration the software includes a powerful option to estimate calibration coefficients the output from calibration for elements that were not calibrated These coefficients will be calculated on the fly for every element that was not previously calibrated The software uses a mixture of fundamental parameters calculations and knowledge about the coefficients of neighboring elements in the periodic table that have been calibrated for the same x ray line e g Ka The standards should be recalibrated routinely at the same SEM settings as the unknown samples to avoid errors from beam current drift and detector geometry variations One method to correct for beam current drift is to normalize the composition to 100 the same is done for standardless analysis Normalization is selected on the Quantitation tab of the Spectrum Properties All of the geometry setup is important for accurate quantitative analysis For example the tilt angle must be included into the geometry setup in order for the software to calculate the correct incidence and take off angles This is accomplished automatically when the tilt angle is entered in the Geometry setup on the Quantitation tab of the Spectrum Properties To use standards with ZAF the following must be done e Create a ZAF calibration file This process is de
154. s on several fields on an image it 1s possible to save the locations using the Save Analysis Positions File button These positions can then be loaded for use on another image with the Load Analysis Positions File button 86 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 6 Working with Spectrum Reports Spectrum Reports tabulate quantitative results from several spectra into a report format The report displays the elemental eN concentrations from the spectra in a table and calculates statistics poles SEM ARF on the concentrations Fast Map A Spectrum Report can be automatically created during the Fast Lines oan analysis of multiple spectra as described in chapter 5 Least Squares Calibration Also a new spectrum report can be created by selecting File New o from the menu A panel similar to the following will appear Stitched Images Stitched Maps YP Mode Spectrum Select Spectrum Report and click OK A panel similar to the following will appear MH Spectrum Report ace C faa Select Data Add Spectra from the menu to add spectra to the report Below is a report with 5 spectra added to it In addition to the elemental concentrations being displayed the statistics Mean Standard Deviation Minimum and Maximum are calculated and displayed H Spectrum Report2 Fs fom Ex Conc Spectrum C Al Si Ti V Cr Mn Fe Co Ni Cu Zn Zr Nb Mo 321 86 126 1 136 12 321 0 351 0 066 402 85 426 0 156 4 079
155. samples by selecting Save Settings from the spectrum properties panel as shown below 79 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 4 16 Material Classification After quantitation the element concentrations can be compared against a given set of materials specifications known as a Materials Classification This is similar to Match procedure except that composition is used instead of spectra The setup of Material Classification is done from the spectrum Properties Quantitation tab shown on the right The Materials Classifications are stored in the Input Database An example of a Materials Classification is the following set of Materials Specifications Fe Fe Material Min Wt Max Wt 316 55 62 302 55 65 313 60 68 Properties IXRF Calibration Std 1 Acquisition Element 1D Quantitation Display Always Quantitate after Acquire Number of Smooths 1 Remove 5i Escape Peaks Remove Sum Peaks Lowest Energy Processed 0 100 Method Auto j Background Setup Method Gauss z Setup z Deconvolution omar Dats RF Quantitation Match Setup Lightest Analyte kV 20 0 Estimate from Spectrum Save Settings Set As Defaut Apply To Load Settings Cr Cr Min Wt Max Wt 12 2 5 3 1 4 3 0 5 1 These are the names of 3 materials Each of these materials has a s
156. specified for normalization in the Quantitation settings Values of 0 for the low and high channels of the Normalization ROI will normalize using the complete spectrum To the right is an example of Background File used normalizing to the whole spectrum When used to strip a peak or peaks with or without a background present specify an ROI that defines that peak Click on the Setup button to setup the background file A panel similar to the following will appear Click on the File button to select the file Enter the Normalization ROI as described above 4 10 9 Selection of Element Analysis Lines When elements are added to the element list for analysis a specific line must be selected which is to be used for quantitative analysis It is this line whose net peak intensity is calculated and used in subsequent analysis e g ZAF Match The user can alter the default selection of lines This can be done in two ways First the default line list can be modified To do this select Setup from the Deconvolution section of the Quantitation tab of the Spectrum Properties as shown here A dialog similar to the adjacent will appear Click on the Element Lines button A dialog similar to the following will appear 49 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 Al J P 3 Cl K Ca ac c PO BR Be A Yh ge J This dialog is used to determine the default lines that will be selected fo
157. stem The spectrum calibration can only be changed by recalibrating the electronics The display can also be used to evaluate the merits of using the linear vs the non linear deconvolution on the spectrum by examining well how each of the methods fit the spectrum And finally if an element is missing in the element list a spectrum peak that has not been fitted will appear in the spectrum but not in the fitted spectrum If Restrict to Linear Peak Fit is selected no information in the Maximum Deviations frame needs to be adjusted If Restrict to Linear Peak Fit is not selected the non linear fitting will be performed In this case there are several adjustments that can be made which will affect the non linear fitting These adjustments are Maximum Iterations Maximum number of iterations for Non Linear Gaussian deconvolution Since this method is iterative this parameter is used to limit the number of iterations If the deconvolution does not converge after this number of iterations the best fit parameters from the last iteration are used Line Ratio Factor The line ratios are allowed to change by up to this factor in order to improve the fit during the iterative portion of the Non Linear Gaussian Deconvolution For example the Ka line is usually about 50 of the Kal parent line In the linear fit the ratio of the Kaz Ka will be fixed to 0 5 in this example For the Non Linear fit assuming a factor of 2 for the Line Ratio Factor this
158. t an entry in the list and click Go To The stage will be driven to the location of the entry The Start Acquisition button is used to start and stop acquisition During acquisition the button label changes to Stop Acquisition Save List and Load List Lists of data to acquire can be stored and recalled If you routinely acquire data e g images spectra fast maps this feature can save the time of setting up the analysis positions The stage locations magnification and other required setup information for acquiring the data are stored in a file when you select Save List These settings can be recalled by clicking on Load List and selecting a file To use RoboStage do the following 1 Select a Sample Name 2 Select how the data are to be stored Individual Files EDS Dataset 3 Move the stage to an area of interest and click on the data that you want Spectrum Image FastMap etc For Stitched Images and Stitched Maps a panel will be displayed to further setup the acquisition Those panels are described in the section on Stitched Images and Stitched Maps 4 Click the Start Acquisition button Turn Beam Off After Acquisition This feature can be used to turn off the high voltage when an acquisition completes In this manner you are not adversely affecting filament life when the microscope is not being used For example you might wish to start a data acquisition run at the end of your workday which might take several hours to acqui
159. t is 100 even though normalization cannot be done This type of component can only be used with ZAF with standards or Match There can only be one diff erence component in the table and normalization cannot be used Once the components have been entered click the Close button to complete the editing of the stoichiometry information Display and printing of the Component calculations is discussed in the section on Customizing Report Output By default only element calculations are displayed and printed These settings can be modified At this time you may wish to save these Analysis Settings for use in the future Use the Save Settings option of the spectrum Properties to store these settings 4 10 2 1 Convert Elements to Oxides A convenient method is provided to convert elements automatically into oxides Clicking on Convert to Oxides will automatically convert the elements to their defined oxide forms Pressing this button will display a panel similar to the following Elements to Convert Select the elements that you wish to have converted to oxides and click OK The elements will be converted to the default oxide forms These default oxides are defined by clicking on the Define Oxides button This is described below 43 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 4 10 2 2 Setup Oxides Panel Use this panel to enter different oxides for each element Type into the Oxide column to change the oxide
160. tailed later in this chapter e Select the calibration file in the Elements Analyzed table of the Advanced dialog selected from the Quantitation tab of the Spectrum Properties Once selected this will be saved in an Analysis Settings file for use in subsequent ZAF with standards analysis 4 13 3 Creating a ZAF Calibration File The ZAF calibration file contains the information primarily calibration coefficients and the critical analysis parameters used by ZAF with standards for analysis Acquiring a spectrum from a standard and processing it with ZAF calibration writes the information to the file The steps are shown below and described in detail 60 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 Acquire Standard Spectrum With the standard in the SEM acquire a spectrum Note the excitation and geometry parameters Set Element List and do Standardless Analysis The net peak intensities for the elements in the standard are needed for ZAF calibration This is why we recommend performing a standardless analysis as this is the easiest way to create the necessary data Ensure that all elements to be calibrated are entered and that the correct lines have been specified On the Quantitation tab of the Spectrum Properties ensure that the spectrum processing Smoothing Si Escape Peak Removal Background Removal and Deconvolution is set properly To verify the analysis lines click on the Advanced button on the Quantitation
161. tandnses 71 4 15 2 Oiantiry ine with east S GUAEECS vccasscspescrasousvornsabtooseauusmantenpeacndeubwasnaehtnnetinanneapecomncerevonncan 77 ALG Maternal Class iCaOMs eccmeccunamosseseiaeamomaestsiiclorses N Ea 80 4 16 1 Enable Materials ClaSSiliCatl OW 1 02 sciersos aca saassansasnmaveactta a e a 81 4 16 2 Select OF Created Daa ds Crespina E EE EE E A E 82 4 16 3 Selector Create a Materials Classon 82 4 16 4 Edit Materials in Materials Class cccccccccecccccsscceessssssseseeeeeesececccssececesssssessseeeeeess 82 4 16 5 Test the Materials Class with Samples ccccccccccccccscssssssssesseeeeccceeeeeeeeeeeaaaaeesesseeseseeeess 83 4 16 6 Setting Minimum Counts in Spectrum ccccccssssseccccceceeeeeeeaeseessseeeeeeceeeeeeeeeeeaaaaagennees 84 4I Spectrum SITU ALON Gs tps gas si cet ca ee tas a eed vets CSS apes S EEE amen EEEE EOE eine SEE 84 Working with Automatic Multiple Spectrum Acquisition ccccccccscssssssssssssssssssssssscscccccccsssssseees 85 S SVS CLIO Local oNu st a a a a a 85 32 Addme Labeled Locations caserie errr EEA A E EA EE EE E 85 5 3 Sclectine Analysis Setin S orele epre e od teen Er ENEE E N Kae a EE EE ENE E TE 86 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 5 4 selectins Location for File SOT ce 2 cuiccdess shir iasianiatenh ite die edanda E a aii 86 5 5 Selecting Report Output Options aisecevics desi satin diniihiead en bicevas dade sates bechiaad ve ee
162. tdadsdenacdacbaatandoudeanstnbaadand aa e 23 3 8 FAG He WICH 5s dceAecasd co aniatnandencassnemnachenaad aacoatetnend mecssawmnasnsanasd enaaiases dma ceuenonstanenoand S 23 oak HERED 2 ccadecsooauansecavenooneimsnsand memactauusa A E S 23 S ADO T A A 23 IS View Reese NO Sorria 23 3 9 Data PROTEC CUON ceinion EEEE 24 Working With Spectra css aa aa a aaa A aa aaa Aa eateries 25 4 1 Acgune SPEC dss eeni aa 26 4 1 1 Returning to Acquisition Location eeeeeeessssssssssseseeererresssssssssssssectrreressssssssssssseeererersssssss 26 4 2 AV IC Wily TOOS prsna hansen dean asanktsepeactchee acisasioamsdeenesareempaeetaatneds 26 4 2 1 Expanding and Contracting Views cccccccccsssssssssssseeecceeceeeeeeeaeaaeesesseesseeeeeeeeeeeeeseeeaaaaaesensees 26 APD AUO METH C ASC ANC x0 ca ansas sccars a e 27 4 2 3 Manual Setting of Displayed Energy eeneesssssssooeeeeeressssssssssssssscrrerreeeressssssssssssseeereeeesssssss 21 ADs Bipolar DISP er e E a e E EENE 24 4 3 Overiivina Specia aens en rE e E a EE teed teed 28 4 4 AMMON ONS and NOES enan n a a E a 29 4 5 Customizing Display and Printing Colors cccccccssssssssssseeeccceeeeeeeecaaseeesessseeeeeeeeeeeeeeeeaaaaaeeeenees 31 4 6 Pamite WNdO WS eere en ra EEEE E Ee E EAE ENER 32 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 4 7 Konyin PC AiG ose sae nacie saa sand sncaamias ne Mies hdsaa ara nen tmeeceetngetemsaaees 32 Sl sElement ID BUON nn S 32 PS R Oe
163. the numbers in the table After setting up the compositions you can process the maps to create the composition analysis map To do this click the Process button Below is the processed image Fe Base 93 6 10 00 100 00 0 00 0 00 Caban 151000 10007 When you click on the image the table to the right of the image displays the value at that point on the map in the Conc column It also displays the minimum Min and maximum Max values for each of the maps This can be useful when determining the min max values for individual compositions 9 14 Scatter Plot Analysis Scatter plot analysis of element maps provides a tool for understanding the relationship between two element maps To begin using this feature select Process Scatter Plot Analysis from the menu An example is shown below of a scatter plot of oxygen vs tungsten concentrations The selected area from the scatter plot is WO3 To use the panel select a map type and the data to be displayed on the vertical and horizontal axis A scatter plot will be displayed Then click on Select Area and use the mouse to 113 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 select a rectangular region on the scatter plot A map of the selected area will be automatically generated o Te FS File Edit Scatter Plot Map Type Element wt Scatter Plot Histogram Selected Area O wt 7 6 17 2 W wt 34 9 68 6 Vertical O wt Horizontal W wt
164. the Apply button will save any changes you have made to this panel Clicking the OK button will save any changes you have made to this panel as well as close the panel Clicking the Cancel button will not save any changes you have made to this panel and close the panel 21 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 This tab contains all the user interface elements that are settable on a system wide scale a picture is shown below Grid Font allows for the selection of a system wide font to be used in the tables of the software Click on the button Font in order to select the font Once a font has been selected a sample will be displayed below the button You must click Apply or OK for any of your changes to be saved once the dialog is closed 3 6 2 System Setup Security This tab contains all security features of the software The panel is shown to the right Password allows for the setting of a system wide password to be used for authentication in sensitive areas of the software Fill in the text box with the desired password in order to set protectanddefend the password You must click Apply or OK for any of your changes to be saved once the Protect dialog is closed V Energy Calibration System Settings Protect allows for setting which areas of the V Image Calibration software are password authenticated Check the appropriate boxes in order to require users to enter a password in ord
165. the angle subtended by the detector with the sample at the origin Itis given in steradians This parameter is calculated by the software Detector is off axis This allows for changing the detector from off axis to on axis For a description of these terms refer to section 4 11 above 4 12 Detector Setup mI a o oo E pam geset m Defi mP Bi a The panel has two sections Detector and Window Parameters The Reset to Defaults buttons in each of these sections will set the default values for the detector based upon the setting for Type in the Window Parameters section Both buttons must be pressed to complete the setup of defaults for a given type Itis important that these parameters be set correctly to obtain good quality standardless analysis especially for light elements in the sample or any element with line energies below about 1 2 keV This information should have been provided by your detector supplier who is the best source for this information 4 12 1 Window Parameters Type This defines the type of window The selections available include common windows from the major manufactures for new as well as older detectors This list is updated as new information is made 57 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 available If your window type is not listed here please contact us for information on a compatible window material Many windows are complex structures with added gr
166. the escape peaks from the spectrum and adds the equivalent original x ray event at the parent peak s energy Method ZAF g Advanced Match Setup Lightest Analyte kv 20 0 Estimate from Spectrum Remove Sum Peaks is only recommended for spectra where a high deadtime was present Itis a relatively time consuming process and is not normally required 1f the deadtime is maintained below about 25 except for low energy lt IkeV x rays where the pulse pileup discriminator is not effective and even modest total count m eee Save Settings Set As Defaut Apply To Load Settings rates can result in peak pileup sum peaks This correction is not as accurate as the escape peak removal and may leave some residual sum peaks in the spectrum Background removal is typically the next spectrum processing step The most commonly used Background Method is automatic Other background removal methods are described later in this chapter The automatic method determines the background using a proprietary technique and then subtracts it from the spectrum Although the exact details of the automatic background removal method are proprietary the method is based on general signal processing techniques that seek to distinguish fast changing regions of the spectrum i e peaks from slowly changing regions 1 e background This is relatively simple for large peaks on small and flat bac
167. the right is the Word document The controls on the toolbar on the right side can be used to directly edit the Word file Place In Report will take the selected data from the tree on the left side and insert it into the Word file From the File menu are the following features Save As Saves the Word document Open Opens a Word document This clears the present Word document and then loads the selected Word file See Insert below if you wish to add an existing Word document From the Insert menu is the following feature Word File This inserts a selected Word file at the end of the Word document right side of panel 18 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 3 5 View Menu 3 5 1 Interactive Help The Interactive Help panel is normally displayed on the left side of the application workspace as shown This panel provides help for using the major functions of the application Clicking on the highlighted text or icon provides detailed guided help for working with spectra images x ray maps and linescans The panel can be displayed or hidden with the button on the toolbar or with the menu item View Interactive Help You can switch from the Interactive Help panel to the Folders panel see next section by clicking the tabs at the bottom of the panel The panels can be auto hidden by clicking on the pushpin icon near the upper right corner of the panel next to the X close icon You can also change the
168. the same as the window material The grids are of various designs which can affect the absorption of x rays on their way to the detector crystal Input the correct value of the support grid thickness in microns as this is used by standardless analysis Windows that use grids include the Quantum and Moxtek windows Certain windows use 2 grids e g the MET4 and Moxtek AP3 3 windows see further parameters described below for the second grid Grid Area Fraction This is the fractional area 0 1 0 of a grid see above used to support the detector window This defines the fraction of x rays that pass through the grid verses those that do not Grid 2 Element This the element used for a second grid that is employed by some window assemblies The MET4 window uses a W second grid The Moxtek window uses a second grid made from BH but this is NOT user definable it is defined internally by the software Grid 2 Thickness This is the thickness of the second grid in microns used by some windows see above Grid 2 Area Fraction This is the fractional area 0 1 0 of the second grid see above used by some windows Reset to Defaults Once a window Type has been selected using this button will reset all other window parameters to the default values for this Type This is useful in getting a reasonable set of starting parameters for the window although you should refer to the parameters supplied by your detector vendor see above 4 12 2
169. the spectrum Panel Orientation selects whether the Spectrum panel and Analysis panel will be displayed left right or top bottom aligned Fonts allows for selection of a font for the spectrum display and the Notes overlay on the spectrum Click on the Font button and a standard Windows font selection panel appears The font and font size can be selected 4 6 Painting Windows A window can be painted on the spectrum to specify a ROI Region Of Interest The ROI can be used for simple integration of an area of the spectrum using the ToolBar button da Window painting is also used when defining Background Model regions Painting is done with the mouse buttons Use the left mouse button to select a region by pressing down the left mouse button and then dragging it across the spectrum As you drag the mouse the selected area of the spectrum will appear painted yellow Lift the left mouse button after the desired area has been selected The right mouse is used to remove un paint parts of the ROI Press the right mouse button down and drag it to erase di Note While Window Painting is active e g during Background Model or use the mouse can only be used to adjust the ROI of the spectrum 4 7 Identifying Peaks One of the first tasks in performing an analysis is identifying the peaks in a spectrum For a qualitative analysis identify the peaks by displaying the element symbols and MLK marker positions on the spectrum For qua
170. the spectrum will automatically add remove the selected element 9 7 Exporting X ray Maps X ray map files can be exported to a wide selection of industry standard image file formats JPEG TIFF BMP etc Selecting File Export from the menu displays a standard file panel with the following additional selections W With Annotations f Mapes exported into one file As Displayed Individual Maps e blaps Export SEM Add 5i Remove Fe Add All Remove All Include Titles The x ray maps can be exported in two basic formats e Inasingle file combining all x ray maps as displayed on the screen e Individually Export into one file To export the x ray maps into a single image file that is similar to the displayed maps select Maps exported into one file Enter a File name and click on the Save button to export the x ray maps Export Individually To export individually select Individual Maps Then select from the Maps list the elements that you wish to export using the Add or Add All to add to the list of exported maps Remove and Remove All will remove the selected maps from the exports list The maps can have titles at the top of the images or not Enter a File name for the images The actual file names will have the element name appended to the file name For example if the file name was TestSample the names of the image files would be TestSample SEM TestSample O TestSample Cr etc Click on the Save button to fin
171. the x ray maps Spot Size can be set to a value larger than 1 so as to include adjacent pixels in the spot intensities The values for Spot Size are 9 8 1 3 Spot 9 8 1 4 Description Size 1 The single pixel at the spot location 9 9x9 grid of pixels The spot location is the center pixel of the grid _ The Save Spot option will store the spot location on the maps create a spectrum file from the spectra at the spot location and add the location to the Locations list Thus the spot data can be reviewed similarly to the Rectangle and Freehand data If Show Spectrum is selected a spectrum for the location will be created and displayed 9 8 1 5 Rectangle Mode When selected the user can select a rectangular area on any of the maps or image After completing the selection the spectra from the selected area are added together A spectrum is created it is analyzed and the intensities or concentrations are displayed in the histogram The rectangle location is labeled and displayed on all of the maps and the image The labeled data are added to the Locations list below the histogram If Show Spectrum is selected the spectrum is created from the area and displayed 9 8 1 6 Freehand Mode When selected the user can select an arbitrary area on any of the maps or image After completing the selection the area is closed by connecting the last pixel selected to the first pixel selected Then the spectra from the selected area are adde
172. ther spectrum to overlay it Do the following Move the cursor over the spectrum you wish to overlay Hold down the Ctrl key and press the left button of the mouse Drag the cursor keeping the left mouse button down until it is over the other spectrum Release the left mouse button then the Ctrl key The spectrum will now be overlaid 3 Select Overlay Copy from the menu of the spectrum you wish to overlay then select Overlay Paste on the other spectrum The spectrum will now be overlaid The overlaid spectra names are displayed in the upper right corner of the spectrum as shown below 28 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 WM IXRF Calibration Std 2 5 10 15 20 keV Right clicking over a name will display a menu Selecting Color allows changing of the overlaid spectrum color Selecting Delete will remove that overlaid spectrum 4 4 Annotations and Notes Spectrum annotations are text shapes that are overlaid on the spectrum The annotations are saved with the spectrum and can be printed exported or copied to the clipboard with the spectrum Text lines arrows free floating text rectangles etc are available to annotate a spectrum These tools are available by selecting Edit Annotations from the menu or by clicking on the button on the ToolBar For instructions on working with the annotations panel please refer to section 4 9 of the Digital Imaging manual Notes are a simple text only
173. tion Area Fe Hin Max Min Max The panel has a menu The menu items are File Load Min Max Settings The composition settings can be saved and loaded to support repeatable processing of maps File Save Min Max Settings This saves the composition settings File Print This prints the image and the composition analysis File Export This exports the image and composition analysis to a bitmap file Edit Copy This copies the image and composition analysis to the clipboard to support pasting into another application Process This starts the processing of the image If concentration maps are required and don t exist they are created as well View Add SEM This overlays the SEM image on the composition maps The composition tool can work with intensity maps element concentration maps or component concentration maps This is selected from the list below the displayed image as shown below Element Concentrations Element Intensities Element Concentrations Component Concentrations 111 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 A map Composition is a set of intensity concentration ranges Map compositions typically relate to phases or element distributions in the sample In this example there are two compositions aluminum stub and nickel grid To begin the composition analysis you must first define the compositions that you wish to view Each composition is added with the Add Composition b
174. tly fit the points An order 3 fit will fit any 3 points to a parabolic curve Below are examples of an order 2 and order 3 fits for Zr Order 2 Order 3 An order 3 fit requires at least 3 points Zero can be one of these points so a linear0 fit with 2 standards is valid Each element can fit either the intensity or intensity Ratio By selecting Ratio for an element the least Squares curve fit will use the intensity Ratio for the element rather than the intensity It is important that the Ratio settings in the standard spectra are also set The intensity ratios calculated during the quantitation of the standard spectra prior to the least squares calibration will be used for the curve fit Below illustrates the ratio setup This can be found in the spectrum properties quantitation panel by clicking on the Advanced button Component Type Mole Conc Units Conc Cr Cale 0 000 0 000 wt Mn Cale 0 000 0 000 wt Fe Cale 0 000 0 000 wt Hements Analyzed Configuration Ratio Setup More Ef Line Ratioed Ratio Ratio Low keV High keV Cc Ka 0O 0 000 0 000 Mn Ka O 0 000 0 000 Fe Ka 0O 0 000 0 000 To setup the calculation of intensity ratios select Ratio for each element and then enter the energy range to use for the ratio Low and High The intensity ratio is then calculated during quantitation as the ratio of the net peak intensity for the element divided by the counts in the ratio region 76 IXRF Systems Inc Iridium U
175. to a variety of file formats including TIFF BMP JPEG Microsoft Word and EMSA The export file options can be found on the File Export menu Also note that the File Save panel has an option to export as well as save the data file This can be very helpful if you both save and export spectra saving the added step of exporting after saving 37 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 Below are the Export options 4 9 1 File Export Spectrum Exports the spectrum to a graphics file format e g TIFF JPEG and also ASCII data formats such as EMSA 4 9 2 File Export Analysis Exports the analysis of the spectrum in a graphics file format or ASCII text format 4 9 3 File Export Multi Spectrum Export Exports all open Spectra to a graphics or ASCH data file 4 9 4 File Export Export to Word i Export to Word Exports the spectrum and optionally the Quantitative analysis and Image associated a i mE Type with the spectrum to a Microsoft Word This folder is empty file Separate heading and footer files can be used to customize the document file These can be used for Company Logo and other documentation purposes The Report Options allows for customization of the output Clicking on the Report Options button displays the Word Report Setup panel as m Ce name shown below E Save as type Word Document do ssi cument doc gt Text Font Clicking on this button allows He for
176. to save the stitched image map Exporting a Stitched Image Map creates a single image map file which can be processed by the EDS software as a single image map If you wish to perform any processing on the stitched image map it is necessary to first Export the stitched image map Select File Export as Stitched from the menu to export the stitched image map For stitched images the File Export as Individual menu item is available This will export each of the images separately to a bitmap file JPEG TIFF etc The names of each of the individual images are suffixed with their row and column numbers respectively 135 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 13 WDX Support Support for a single WDX channel input for FastMaps and FastLinescans is provided as an option to the EDS software When this option is enabled as shown below the WDX1 signal input can be selected Default Xray Map Propertis pS He us BOC NO F Ne Na Mg Al Si P S Cl Ar K ca sc Ti V E co zn Calel As Se Br Kr Rb Sr Y Zr Nb Mo Te Ru Rh Pa Ag Ca In Sn Sb Te 1 Xe Cs Ba La Hi Ta W Re Os Ir Pt Au Hg Ti Pb Bi Do At Ro Ce Pr Nd Pm Sm Eu G4 Th Dy Ho Er Tm Yb Lu Th Pa U Np Pu AmC Bk Cf Es Fa When this option is selected a map linescan will be acquired from the WDX signal The WDX signal is not used in the quantitation of maps linescans but is available for all display functionality
177. tration are displayed as points on each graph As you can see some of the graphs show the curve fit passing through or very close to all of the points C Si Ti V Cr Mn and Ni are examples of these good fits Other curves have points that are above or below the curve Examples of these are Al Zr and Mo of fits that are not as good The points that are used for the curve fit are colored blue Points that have been removed from the curve fit are colored gray 0 S40 100 150 200 250 300 Cts Core 0 090 Titers 65 41 Stardard oo2 Clicking on an individual point on a graph will display the standard name concentration and intensity for the point If you want to remove a point from the curve fit for a particular element right click over the point in the graph A menu will appear Select the menu item Remove X where X is the standard name Below is an example File Edit Remove Standard 662 O 50 100 150 200 450 300 Cts Core 0 090 Titers 65 41 Corc Stardand 002 Starula After removing 662 from the fit this is how the graph is displayed Notice the grayed point This is the standard 662 which is no longer included in the curve fit for aluminum 0 0 100 150 200 250 300 Cts To add the standard back into the curve fit right click over the point as before and select Add X from the menu where X is the standard name 74 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 4
178. trum Delete Windows 0 735 0 825 Ceara 0 1 205 1 285 ae 0 a B 0 135 0 175 1 0 335 0 375 Open Save peta bosdi Properties IXRF Calibration Std 2 e S OK Cancel Acquisition Element ID Quantitation Display Now you can save the model as Means Caa aie Aa a win file This can then be acto uk Seca used to specify the background model for Quantitation To do this select the Background Method as Model on the spectrum Properties Quantitation tab as shown Then click on the Setup button v Remove Si Escape Peaks Remove Sum Peaks Lowest Energy Processed 0 100 Background Method File 7 Background Setup Click on the File button Fie and select the model file Nomalization ROI 0 000 jg 9 000 48 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 4 10 8 Background File The Background File method uses a stored spectrum file as a means of estimating and removing the background This spectrum file should have the same general shape as the background in the sample spectrum which implies that the sample should be similar in composition and the excitation kV should be the same Since the stored spectrum could have peaks as well as background the technique can also be used as a peak stripping method Prior to subtracting the background the stored spectrum should be normalized to the spectrum A region of interest ROT in the spectrum must be
179. trum Properties E n 51 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 Note these settings revert to the default lines if the element is removed from the element list and then subsequently added To re apply the settings to a spectrum use the Load Settings button 4 10 10 Gaussian Deconvolution Gaussian deconvolution fits gaussian shaped peaks to the spectrum as a means of determining net peak intensities from the spectrum All peaks for all relevant lines for all elements on the element list are fit to the spectrum The kV of the spectrum will limit which lines K L M are actually used For example if the spectrum was acquired at 5 kV and Fe is on the element list only the L series lines for Fe will be fit because the K series lines for Fe are above 5 kV More specifically it is the line series edge e g K or L III that must be below the excitation kV Usually a margin about 1 kV is added to this otherwise the ionization probability would be too low to be useful Thus it is very important that the kV be entered correctly for the spectrum If you are unsure of the kV of the spectrum you can view it by selecting Spectrum Info from the View menu Another check on the kV is to observe the high end of the spectrum background which should end just above the kV value because of detector broadening Two kinds of fits are provided Restrict to Linear Peak Fit This allows only the peak height to be adjust
180. ts the spectrum Vertical Scale Expands the spectrum horizontally F to DRE Compresses the spectrum horizontally Enables display of the energy cursor on the spectrum Enables the painting of an ROI on the Performs Automatic Element spectrum Identification Erases Automatic Element Identification Displays the Periodic Chart for manual element identification Toggles display of Spectrum Analysis Report Enables annotation on the spectrum or Performs Quantitative analysis of the image ae spectrum Selects a new set of default analysis settings Displays or Hides Interactive Help fay Image selects spot location Linescan selects horizontal line For images selects a freehand area for acquisition of a spectrum For linescans selects an arbitrary line _ For images selects a reduced raster area on the image for acquisition for acquisition of a spectrum For images selects an area for For images selects a line for acquisition acquisition of an x ray map of an x ray linescan 1 panel TOE isles ee minic IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 The bottom half of the ToolBar contains controls and status readouts used for acquiring data These controls are described below g Acquire Preset 10 0 Livetime Livetime 10 0 0 gs TG 1 0 kV 20 0 Mag 100 Active Stage Microscope Stage Acquire ee a Acquire Start Stop This bu
181. tton starts and stops acquisition on the active window e g Spectrum Image X ray Map During acquisition the button text is changed to Stop to indicate that the action taken when the button is pressed is to stop acquisition Preset 10 0 Spectrum Preset Value This is the preset value in livetime seconds or total counts in the spectrum Acquisition will automatically stop when the preset condition occurs The Spectrum Preset Mode determines whether the value is livetime seconds or counts Livetime ka Spectrum Preset Mode This selects the kind of Preset to use For Livetime the spectrum is acquired for the given number of seconds of livetime For Counts the spectrum is acquired until the specified number of x rays has been acquired total counts in the spectrum ivetime 10 0 a ooe po Spectrum Acquire Livetime During acquisition of the spectrum this control displays the livetime seconds This is the clock time that is corrected for deadtime Spectrum Deadtime Meter This continuously displays the deadtime percentage A bar graph and a numeric readout are displayed Deadtime is the time that the pulse processor is unable to process incoming x ray events as it is already processing a prior event i si Spectrum CountRate This continuously displays the input countrate E 1 0 ba l E Time Constant The time constant can be set directly from here This is the time constant that will be used for all subsequent data acq
182. tween the major lines that will cause some lines 1 e the ones above the edge to be preferentially absorbed Therefore it is advantageous to allow these ratios to change depending upon the sample spectrum However if the ratios were allowed to be completely ignored non linear fitting will often produce completely erroneous peak fitting where the fitting error 77 is small but the solution is completely bogus even negative peak heights may result To avoid these kinds of solutions we only allow the line ratios to change by certain factors with respect to the most dominant line The default factor is 2 0 which means for example that the KB Ka ratio could change up or down by a maximum of a factor of 2 0 from the default line ratio stored in the software So if the KB Ka ratio started at 0 1 the maximum allowed would be 0 2 and minimum would be 0 05 This is known as constrained fitting Similar constraints are applied to the fitting of the peak widths and position centroid locations X ray peak resolutions are a well known function of both the peak energy and the system resolution typically for the Mn Ka peak So again the fitted peak widths are constrained to conform to this equation within certain limits The default variation for each peak is 35 For example if the peak had an initial predicted resolution of 200 eV the maximum allowable width for this peak would be 270 eV and the minimum would be 130 eV Similarly for
183. ue to the rapid LESA LEIS 6 5 movement of the beam over the area being mapped 5 772 6 026 6273 6535 Acquisition Bement Selection Quantitation Setup Palettes SEM Palette Time Constant is set separately for spectra x ray maps and x ray linescans The Time Constant appropriate for this x ray map see Preparing the microscope and EDS system for acquisition above for details should be set here Also see the note under Point Dwell above about appropriate settings of Point Dwell and Time Constant Overay Settings Rg es a a None Smooth 11 Median Filter 2 Auto Level after Filter Map Recovery is a feature used during acquisition which makes Transparency a backup copy of the acquisition which can be used if the acquisition is abnormally terminated To setup Map Recovery select Enable and a backup period Backup Every If the map acquisition terminates abnormally restart the EDS software and immediately select Tools Recover Fastmap File from the menu Note starting a new FastMap acquisition will erase any previous recovery information so it is very important to recover the FastMap file immediately upon restarting the EDS software Set As Defaut Save Settings Load Settings 9 2 1 Returning to Acquisition Location The microscope stage location is stored at the start of acquisition To return the stage to the l
184. uisition spectra x ray maps x ray linescans Ee Microscope kV Enter the accelerating voltage kV of the microscope in this box prior to acquiring a spectrum X ray Map or X ray Linescan This value is used by the software to control the analysis of the acquired data It is very important that this value be entered prior to acquiring the data On systems with microscope control the kV is automatically read from the microscope Mag 100 ee tesa er a Microscope Magnification Enter the magnification of the microscope in this control prior to acquiring an Image The value in this control is stored in the image at the beginning of acquisition of the image All image measurements are based upon this value so it is very important that it be correct for any measurements to be calculated correctly On systems with microscope control the magnification is automatically read from the microscope Active Stage Microscope Stage oo Active Stage For systems with an IXRF Super Stage or other supported secondary stage the active stage is selected here The active stage is used for image and map stitching and stage maps and stage linescans The full stage position is saved with all data acquired with 12 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 the EDS software both active stage and microscope stage This allows for accurate repositioning of the stage s to review acquired data locations 3 3 Men
185. us A unique menu is displayed for each kind of window There are however some common menu items that are applicable to all windows These are described below Throughout this manual references will be made to items on the menu The style will be Menultem SubMenultem Menultem appears on the menu directly at the top of the application and when the right mouse button is clicked over a window e g Spectrum X ray Map Selecting Menultem will display a drop down sub menu For example the menu shown below for the Open submenu item on the File menu would be referenced as File Open 3 4 File Menu The File menu is shown to the right All of these menu Che eee Ee items are common to Spectra Images X ray Maps and New Ctrl Linescans Notice that an icon picture is displayed to the Opens Ctrl C left of some of the menu items The icon is a reminder that Import this menu item is also available from the ToolBar by pressing the corresponding button Set Sample Mame Image Browse The menu items listed below Print Setup are special eS er These menu items are numbered 1 2 3 etc and have a file Setup Export File Formats name next to each of them These are the most recently Print Setup opened files Selecting one of these will automatically open 1 100maqg irnx the file as if you had selected Open from the menu 3 4 1 New Creates a new active window e g Spectrum Image A panel similar to the followin
186. usessatensesaadedasesassgsataadeuaasatensesaadedaneasgaasaadesaoonatebaataededanewaaebetdedescoeces 115 9 17 1 SD COMMON Pane ieissar E EEE bored EEEE 117 ae ae Color Control Pane hw scacaansconeccandsnanannsihe EE EEEN A 118 9 17 3 Zoom ONO lh PANE Ferseni on E E EN A O 119 9 17 4 DD N oera E A EE E omg ane bein acne Aun 119 OAS Ata Wap Die CONECO eE E EE E EE E E 119 9 18 1 Enablne DACON Cl OW senyeres SS 121 9 18 2 Acquiring Maps with Drift Correction eeeesssessssssseeeeeerreessssssssssssseeerrressssssssssssseeeeeeeee 121 10 Working with X ray Linescans sssesssseseccccccceccccccssoccsoccccccceccccccocecosecceseccececeecocosossesecccccecceeceeeee 123 IOF Acgurme Xray LAMCSC all ccs eae T aa 123 10 1 1 Preparing the microscope and EDS system for acquisition cccccccceccccssssssseeesseeeeeeeees 123 10 1 2 Creating and Acquiring the X ray linescan ssosssssseoooeeeeeeessssssssssssseerreeresssssssssseseeeeeeee 124 10 2 Setting Acquisition Properties sessies i iretsi ariii spar ennir rinii ye cent Dies denddparieweapereerderd tend 124 10 2 1 Returning to Acquisition Location sesesssssssssseeeeeterressssssssssssseeesseererreressssssssssseeeeeeeee 125 LOS Settings Element Propere Sx eis Seat a ronpi cine ES EEE NE E ve ean NEKEEN EERS EEEE KENEEN 125 LOA Viewine Intensities amd Concentra onser enea a a aunt ean ae eae 126 IOS SOV ETA VDSS CAINS arser n EE teramatevantee ea eutenstatuac Oa vementoo
187. utton Clicking on the Add Composition button will display a panel similar to the following Description Fe Basel The description can be any text In our example we use Fe Base Each composition must also have a color associated with it This will be the color that will be used to show the composition on the composition map Click on the Color button and a panel similar to the following will appear Basic colors al ey eee ens Fe Fe ee Oe i an NEENEHE A A BEE EE E taeserenrene Custom colors BEE EEE ee i it i i i Define Custom Colors gt gt m Select a color for the composition from this palette of colors Itis best to select colors that are distinct from the other compositions that you are defining for this sample Below is the completed list of compositions for the sample Composition Description Area Fe C 4 Min Max Min Hax Oee Fe Base 0 0 0 00 0 00 0 00 0 00 ae Carbon 0 0 0 00 0 00 0 00 0 00 Now we must set up the ranges min max for the compositions To do this enter the numbers in the table Below is an example for this sample 112 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 Description Area Fe Base 0 0 Carbon 0 0 0 00 0 00 10 00 100 00 For a composition it is not necessary to have all element ranges specified In this example only Fe is defined for the Fe Base and only C is specified for the Carbon This is indicated by the color of
188. utton If you do not wish to complete the calculation and display of concentration data you may press the Cancel button Clicking on another location on the linescan will display the concentration at the newly selected point 127 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 10 5 Overlay Linescans Linescans can be combined and overlaid on the SEM image using the View Overlay Linescans menu item A panel similar to the following will appear when this menu item is selected Color eq Basic colors The Elements list contains all linescans that can be combined To adda _ el ae linescan select it from the Elements list and click on the gt button E Another way to add the linescan is to double click it A panel similar to the following will appear Select a color for the linescan A EE EERE Eee After selecting a color the combined linescan on the right side of the EEE E panel will be re displayed with the selected element added Custom colors EEE EE ff BEE u d ee Define Custom Colors gt gt e This procedure can be repeated to combine other element linescans Below is an example of a combination Ca Overlay X12 The panel can be re sized making the graph larger or smaller as desired With the mouse grab a corner of the panel and drag it to change the size of the panel 128 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 Elements can be removed f
189. vailable including TIFF JPEG and Windows Bitmap 3 4 13 Print Prints the active window 3 4 14 Print Preview Displays the active window as it will be printed This can be used to preview the printed data prior to actually printing it 3 4 15 Print Setup Provides Windows standard printer setup A selection of printer and printer options is provided 3 4 16 Exit Closes all active windows and exits the EDS application 17 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 3 4 17 Create Word Report Displays a panel similar to the following Word documents can be created and saved using this panel All presently opened images spectra x ray maps and x ray linescans can be inserted into the document as well as analyses generated from the data Note this requires prior installation of Microsoft Word 2000 or newer software on the computer that is running our EDS software T Create Microsoft Word Docun File Insert EDS Data Home Insert Page Layout References Mailings Review View Acrobat E B X Calibri Body 11 33 B T U abe x x Paste ab A TS a SE Quick Change Editing wr E dk Aar A A ale Styles Styles T L Fast Linescan Clipboard Font F Faragraph Styles Spectrum Report Combined SEM ARF Spectrum Eal JWP Mode Spectrum a ie The tree on the left side of the panel displays all of the opened data The panel on
190. ve a name next to each of them These are the windows that are presently opened in the EDS application The active window has a check next to it Selecting one of these will ain Arrange Icons make it the active window 2 Imagel 3 FastMapl 4 FastlineScanl 3 7 1 Cascade Windows Rearranges the windows in a cascading manner 3 7 2 Tile Rearranges the windows in a tiled manner All windows are displayed in equal sized rectangles in the EDS application window 3 7 3 Arrange Icons Rearranges the windows that have been minimized on the bottom of the EDS application window 3 8 Help Menu The Help menu is shown below All of these menu items are common to Spectra Images X ray Maps and Linescans Help Topics P About View Release Notes 3 8 1 Help Topics Displays a list of the Help Topics for the software 3 8 2 About Displays information about the application version and the available installed EDS options 3 8 3 View Release Notes Opens the release notes file doc file for the application 23 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 3 9 Data Protection Data Protection provides two mechanisms to ensure that acquired data is not mistakenly lost during normal operation of the software These data protections are enabled by default but can be disabled L Whenever a window is closed and the data acquired in the window has not been saved the us
191. vers g H E I 1386 Intel C3 IXRF IXRFDATA 3 Backups 1 17 08_coupon 1 Leds E8 2 Limx E 2 2 imx fi 2 3 x8p ra 3 1 imx fl 3 2 imx 3 3 mpF Po ra 4 Limx E 4 2 imix E 5 micron new pelle B 210ct09 xsp 30455 x5p 651 sp i 663 xsp E Basic Mi Grid imx CRF Lhi nAn sa gt Ltt Interactive Help Folders Ready IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 3 5 3 Application Look The Application Look menu item is only shown when the EDS application is initially pms opened and there are no data displayed Interactive Help where only a blank workspace is visible This Status Bar _ menu item can be used to change the Application Look gt Office 2000 application appearance to suit the user s Office XP preference See Again note there are no spectra images x T ee ray dot maps or linescan profiles displayed P Office 2007 Visual Studio 2008 Visual Studio 2010 a i Blue Style Black Style Below are some examples of different application looks Office 2010 Black File View Tools Office 2007 Aqua i File View Tools Help 3 6 Tools Menu The Tools menu is shown below See Chapter 11 of this manual for RoboStage information and the separate PA PDF manual for particle analysis information 10 pt Times New Roman Tools Window Help RoboStage Particle Analysis System Setup 3 6 1 System Setup User Interface Clicking
192. volution process of complex overlapped peaks easier 143 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 To measure the FWHM 1 Select the FWHM tab On Energy Calibration the Energy Calibration p anel A panel similar to Automatic Manual Advanced FWHM Low Energy Calibration the following will appear i cha Peak Center 6 900 a erations 10 2 Witha pure Mn sample aai ae eM 01 Start acquiring a Mean spectrum Adjust the STD Update System FWHM count rate such that it is Calculation Method approximately 1000 c s Print Co ee Calculate At Cursor counts per second i ee 3 Set the acquire time to i 100 seconds for the spectrum 4 Ensure that the Peak Center on the FWHM panel is set to 5 9 This is the approximate peak center energy for the Mn Ka peak Ensure that Iterations is set to the number of repetitions of the measurement desired The default is 10 It is recommended to use at least 4 The field Threshold may contain any value between 0 and 1 excluding 0 and 1 the default value is 0 1 This value is used to calculate the Full Width at Threshold Max FWThM For example if the Threshold field contains 0 1 then it will calculate the Full Width at Tenth Max Though the calculated result is not used by the software and can be ignored for all energy calibration purposes the ratio between the FWThM and the FWHM is very useful in determining detector quality and calibration 5 Click
193. wt 6 Steel ff C EF He steell fpe At this point quantitative analysis with these settings will now use the ZAF calibration file It is a good idea to save these Analysis Settings so that they can be used to analyze samples in the future using ZAF with standards Once saved these settings can be set as the default settings by selecting Set As Default on the Spectrum Properties dialog or by selecting them from the button on the ToolBar They can be loaded at any time with the Load Settings button on the Spectrum Properties 4 13 5 ZAF Warnings and Errors After a ZAF analysis any warning or errors detected during the quantitation are displayed at the bottom of the analysis The text always begins with the following line 65 IXRF Systems Inc Iridium Ultra Software User s Manual Rev 1 4 Warnings and Errors Below is an example of an analysis with two warnings displayed Eit Line Intensity Error Cone cfs 2 sig Cr Ka 1138 50 55 256 17 701 wi bii Ka g7 62 21 580 1 171 wh Fe Ka 2709 01 82 610 69 172 wt Hi Ka 309 59 30 878 11 956 wt 100 000 wt Total E 20 0 Takeoff Angle 3307 s tWarnings and Esrors Warning Moa Calibration File for Win Warning Elements not in specified Calibration File Mi The following are the possible error messages and a description of each message Error ZAF not enabled or missing from software The ZAF software is either not enabled with the HASP plug or has failed to load with the a

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