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Ibex User Guide

1. Click once on an element and then click Delete Label e Display peaks with a minimum intensity Threshold Display element lines with relative intensities above a defined threshold in the peak hints and peak identification Click Threshold select an intensity value and then click OK Relativity Intensities EJ e 5 100 200 300 400 500 600 700 C 800 300 1000 3 Applv the changes to Peak Hints Click Close Peak Information Display information about the peak that the cursor is located on 1 Move the cursor to a peak 2 From the View menu click Cursor Place the cursor on the peak you wish to view information on by clicking once on the peak 2 12 IbeX MAXray User s Guide 136826003 2 Using IbeX MAXrav Labeling a Spectrum 136826003 From the View menu click Peak Information Bkgd Left keV Energy 1 742 keV Counts 2221 cts Bkad Right 1 762 keV Intensity 740 Cps Resolution 89 ew Peak Bkad 61 563 Close The Background energy to the left and right of the selected peak displays in the Bkgd Right and Bkgd Right fields The Energy Counts Intensity Resolution and Peak Bkgr values display Modify the peak information location range Enter a value for the Bkgd Left and Bkgd Right and then click Compute The peak information for the energy range displays Exit Peak Information Click Close Displaying KLM Markers Add KLM labels
2. The scans maximum energy level in keV Step Size The spectrometer step size during acquisition in eV 2 22 lbeX MAXray User s Guide 136826C03 2 Using IbeX MAXrav Setting Up a Scan Acquisition 10 Dwell Time The dwell time on each step in seconds Detector Bias The optimum detector voltage for the scan range SCA Baseline The optimum detector baseline voltage for the SCA scan Bv optimizing this value vou can reject counts produced bv noise SCA Window The optimum range of detection for the SCA scan in volts Bv optimizing this value vou can reject counts produced bv noise The sum of SCA Baseline and SCA Window must not exceed 8 4V Save the defined parameters Click Save to save the set of parameters Click Ves to confirm the save command Click Restore All to reset to the systems default settings The bias settings and the ele ment table are reset Click Yes to confirm the reset all command This resets all the scan parameters to default settings only use this option in the case where most parameters need to be reset Click Restore Be Bervilium to reset the current element only This buttons name changes each time the current element changes and only resets the current element Apply the changes to Scan Parameters Click Close Apply the changes to Setup Scan Click OK to save the changes and exit Click Cancel to exit without saving the changes Saving the Acquisition
3. ken Ooo Slider Drop Down Box A drop down box contains an arrow that displays a list of available options Click on the arrow button to display the list and then select an option Open a WDS Spectrum File Look in E data v Drop Down List IbeX MAXrav User s Guide 2 3 2 Using IbeX MAXrav Software Controls and Lavout Check Boxes Click a check box to choose the corresponding option and check mark displavs Click on the check mark to remove the selection The example below shows several check box options Only one is not selected Acquisition Information Ix IV File Name C Noran wDS datakw Si wdx SS Check Box M Title Aw Particle on Si M Date Wednesday May 19 199 en IV Sample EEE IV Time IV Identification i mi ed No Comment F Diffractor PET o V Microscope peores 0 IV Begin Scan b 1700 ke M Beam Voltage fo IV End Scan 1 825 keV M Beam Current fin M StepSie 0 002 keV IV Spot Size regi W Dweltime 30 IV Aperture B R TotaPoints 63 IV Magnification Raster 40K Detector Bias 2050 volts IV SCA Baseline 1 00 volts I SCAwindow 600 yalts Close Option Buttons Only one item can be selected from a set of option buttons Click one option button and the other item s are no longer available The example below shows 4 sets of option buttons From each set only one options can be selected Modify Display xl Plo
4. 136826C03 verifv the remaining fields e X ray Line K L or M line Diffractor The diffractor Peak The peak centroid location Bkgd 1 The low background count location Bkgd 2 The high background count location Standard The standards element defined during element setup Standard Time The amount of time to acquire the Standard Unknown Time The amount of time to acquire the unknown element Beam Current The beam current acquiring standards Area Peak Factor Adjust for changes in a peaks shape in carbon analysis Select the Peak Search Parameters Both options can be selected Any edits you make in this area display in the Peak Search dialog box For more information see Peak Search Select On Std to preform a peak search on the element at the designated energy val ues Select on Unk to preform a peak search on the unknown element at the designated energy value Begin the acquisition Select one of the following acquisitions buttons Click Start to acquire all elements starting at the beginning of the list e Click Acquire One to start and stop after acquiring the currently selected highlighted element e Click Continue to acquire element in the list starting at the currently selected high lighted element and continue through the list in the order they appear The following prompts display to verify set up information Acceleration Voltage Po
5. Changing Displav Colors Customize the displav and spectrum colors with the following procedure 1 From the Options menu click Change Colors Change Colors Ix p Spectrum p Text 1 Background Peak Labels Numbers Overlay 1 Suround KLM Markers Axis Labels gie sm Karin meta Overlay 2 Border Sun mel r Default Color Schemes Yellow Blue Red White User Default Save Default Close 2 Setthe color scheme Click an item button and then select a color Select from the following items or select a preset default color scheme Spectrum The spectrum line or histogram Overlay 1 The first overlay spectra Overlay 2 The second overlay spectra Background The color behind the spectrum Surround The area surrounding the spectrum window Border The area around the spectrum window Peak Labels Display over the spectrum KLM Markers The KLM markers Numbers The vertical and horizontal scale numbers and tic marks Axis Label The axes labels Default Color Schemes Yellow Blue A preset color scheme using yellow and blue Red White A preset color scheme using red and white e User Default The defined default color scheme 13682603 IbeX MAXrav User s Guide 2 9 2 Using IbeX MAXrav Labeling a Spectrum 3 Applv the changes Click Close Customizing the Default Color Scheme The default color
6. Click the lt and gt button or click and drag on the spectrum to move left or right with the right mouse button Vertically Scale the spectrum Click the A and v buttons or click and drag on the spectrum to move up and down with the right mouse button e Move the arrow buttons to the desktop Click and drag on the blank area around the arrow buttons The arrow buttons are on a toolbar to provide additional display area 136826003 IbeX MAXrav User s Guide 2 7 2 Using IbeX MAXrav Displaving a Spectrum The IbeX MAXray window shows the energy keV and number of counts at the cursor position You can drag the cursor across the spectrum Display Options Determine the information to view in the IbeX MAXray window Select from the following options 1 From the Options menu click Modify Display Modify Display Ix Plot 5 Color e U ni Color C Line Black amp White r Data Font C Raw C Thick Smooth Thin 2 Select Display Options Select one option from each section Plot Display the spectrum as a Histogram or Line e Color Display the spectrum in Color or Black amp White Data Display the spectrum with Raw data or with Smooth averaged data Font Display text in a Thick bold or Thin regular font 3 Exit Modify Display Click OK to save the changes and exit 2 8 IbeX MAXrav User s Guide 136826C03 2 Using IbeX MAXrav Displaving a Spectrum
7. 2 1 Specimen 2 25 Spectral Acquisitions 2 28 Display 2 7 Graph 2 28 Spectrometer 3 3 Index 4 IbeX MAXrav User sGuide Spectrum Labeling 2 10 Saving 2 29 Spot Mode 2 16 Spot Size 2 17 Standards 2 30 Results 2 38 Setup 3 6 Starting Acquisitions 2 28 IbeX MAXray 2 5 Scans 3 3 the Svstem 2 6 Status Bar 3 4 Step Size 2 20 2 22 Stoichometry 2 30 Stopping Acquisitions 2 28 Scans 3 3 Sum of All Counts 2 28 T Threshold 2 15 Title 2 16 Tool Tips 3 4 Toolbar 3 4 Total Counts 3 3 U Unknown Elements 2 34 3 7 User Scan Buttons 2 23 V Vertical Scaling 2 7 Scrolling 3 5 View Menu 3 4 IbeX MAXrav User sGuide Viewing Overlavs 3 5 Results 3 7 Voltage 2 16 3 4 W Warnings 1 1 WD Spectrometer Controller 1 5 WDS 2 6 WDX 2 29 WDX EMSA 2 6 Weight Percent 2 30 Window Protection 1 7 Windows Tools 2 2 X X axis 2 28 Y Y axis 2 28 Z ZAF 2 38 Index Index 5 Index IbeX MAXrav User sGuide Index 6
8. Bias voltage SCA Baseline voltage and SCA Window voltage must be determined 1 From the Settings menu click SCA Scan Single Channel Analyzer Scan LLD pi volts End 4 volts Step 2 volts Dwell 1 0 sec Window fo2 volts Bias 2300 7 volts T T T T T T kin 20 30 40 50 60 70 80 Close Window Noise Peak 2 Begin the scan Enter the Bias voltage and Low Level Discriminator LLD and then click Start LLD The voltage setting that prevents the noise peak from displaying Bias The voltage determined during in the bias scan Use the system default settings for all other parameters 3 Determine the correct SCA voltage 2 18 IbeX MAXrav User s Guide 136826C03 2 Using IbeX MAXrav Setting Up a Scan Acquisition e The SCA baseline occurs at the valley between the noise peak and the start signal peak s The SCA Window is the peaks width from the baseline voltage to where the peak tails off 4 Exit Single Channel Analyzer Scan Click Close Scanning for One Element Scanning for a particular element with the 1 From the Acquire menu click Element Scan ce Pr Na Pm sm Eu Tefov Ho er Tm yo Lu a Pal U No Pufa e e E nuj 7 User Defined Scans gt Color User Scan 1 User Scan 4 C by X Ray Lir User Scan 2 User Scan 5 by Diffractor User Scan 3 User Scan 6 Cancel 2 Select an element Click once on the eleme
9. Delete Remove an element from the standards setup list Click once on an element then click Delete e Clear All Delete all the elements from the standard 5 Save the standards file Click Save 6 Exit Setup Standards Click Close Acquire Standards Acquire the counts for the selected elements Before defining an element enter the composition of the element s Setup Standards While acquiring standards it is assumed that the beam current is stable and the value is measurable Background regions are defined on either side of the x rav peak The background energy is counted for 1 2 the peak time Standard Counts Gross Peak Counts Background Counts The standard counts and counting errors display when the count is finished The status bar at the bottom of the window displays the progress of the count for an element 136826C03 IbeX MAXrav User s Guide 2 31 2 Using IbeX MAXrav Quantitative Analvsis 1 From the Quant menu click Acquire Standards Acquire Standards Kal WSi60 0 0 469 0 60 11 024 154734 a 591 oxygen Si Kal PET 1 621 1 878 silicon 60 10 917 44204 210 2 Edit or Insert elements Click Insert or Edit and then click Table to select the element Edit Acquisition Parameters FE The following fields displav Select the Standard element from the drop down list and 2 32 IbeX MAXrav User s Guide 13682603 2 Using IbeX MAXrav Quantitative Analvsis
10. Open 3 1 Open Overlav 3 1 Overlav 1 3 1 Overlav 2 3 1 Save 3 1 Save As 3 1 Open EMSA 3 2 Save as EMSA 3 2 Print 3 2 Print Options 3 2 Print Preview 3 2 Exit 3 2 Edit Menu 3 2 Acquisition Information 3 2 Scan Parameters 3 2 Acquire Menu 3 2 Element Scan 3 2 Setup Scan 3 3 Peak Search 3 3 Start Scan 3 3 Stop Scan 3 3 Pause Scan 3 3 Count Menu 3 3 Rate Meter 3 3 Counter 3 3 Settings Menu 3 3 Configuration 3 3 Position Spectrometer 3 3 Bias Scan 3 4 SCA Scan 3 4 Beam Current 3 4 View Menu 3 4 Cursor 3 4 Peak Labels 3 4 KLM Markers 3 4 Peak Information 3 4 Status Bar 3 4 Toolbar 3 4 Tool Tips 3 4 Contents Vertical Arrows 3 5 Horizontal Arrows 3 5 Overlav 3 5 Overlav 1 3 5 Overlav 2 3 5 Options Menu 3 5 Smooth Spectrum 3 5 Scale Spectrum 3 5 Scale Overlav 3 5 Offset Overlav 3 5 Identifv Peaks 3 6 Peak Hints 3 6 Clear Labels 3 6 Select Labels 3 6 Modifv Displav 3 6 Change Colors 3 6 Sound 3 6 Quant Menu 3 6 Setup Standards 3 6 Acquire Standards 3 7 Acquire Unknowns 3 7 Acquire Peak to Background 3 7 Results 3 7 Service Menu 3 7 Initialize Motors 3 7 Password 3 7 Help Menu 3 7 Introduction 3 7 Navigating 3 7 How To 3 8 Menu Commands 3 8 About 3 8 1 Precautions and Safetv Summarv Safetv Precautions 136826C03 Labels and documentation for the IbeX MAXrav indicate safetv precautions as a WARNING or CAUTION WARNING is used when the hazard or unsafe practice could result in
11. Print to print the currently displayed element information Matrix Correction and Linear Regression Matrix correction is used during analysis except when the same element is used 2 times in an analysis The Analysis type automatically changes to Linear Regression Follow the steps below for a linear regression 1 Define 2 standards using the same elements but different concentrations IbeX MAXrav User s Guide 2 41 2 Using IbeX MAXrav Quantitative Analvsis 2 Start an acquisition by loading the same element and use the 2 standards defined in step 1 the example below shows the same element using the 2 different standards Acquire Standards Procedure None Analysis Type Linear Regression Beam 10 0 kV Tilt jo deg Azimuth 0 deg Peak BkgdLo BkgdHi Time Beam Standard Count Element Line Diffractor keV keV keV Standard sec nAmp Counts Error B Kal MoB4C200 0 185 0 154 BPSG_A 1 000 B Kal MoB4C200 0 185 0 154 0 231 BPSG_B 60 1 000 il rm Procedure r Edit Data Acquisition l Load Std Edit Start Stop Save Std Print Delete Continue Pause Acquire One Results Close Ready 3 After acquiring click Results Microsoft Excel opens To confirm that you want macros enables click Enable Macros An new Microsoft Excel spreadsheet displays with a button labeled Read Data Click Read Data to display the linear regression graph and data 136826C03 2 42 Ib
12. menu click Beam Current Measurement 6 948 nAmps M Smooth Bear Specimen Quantitative Analysis Options Mm Feredey Cur I Amp Meter eee 2 Selecta reading location The beam current reading is obtains from the Specimen or Beam e Specimen Reads at the stage level use input 1 if you have the optional current meter equipment Beam Reads at the beam current with an automatically inserted Faradav cup 3 Select the Analvsis Options Determine the analvsis option s to select from the following table Faradav Amp Meter Outcome not selected not selected Manually insert the Faraday cup and Manually record the current not selected Selected Manually insert the Faraday cup and automatically mea sure the current via input 1 Selected Selected Automatically insert the faraday cup and read the current via input 2 Selected not selected Manually insert the Faraday cup and manually record the current 136826C03 IbeX MAXrav User s Guide 2 25 2 Using IbeX MAXrav Setting Up a Scan Acquisition 4 Start the beam current reading Click Start The beam current displays and continuously updates To average the reading click Smooth 5 Stopthe reading Click Stop Peak Search Peaks shift due to other element or chemical structure A peak search locates a peaks centroid or locates a specific elements peak The Peak Search is an automatic operation during Quant
13. scheme is applies to all new files Edit and applv the default color scheme with the following procedure 1 Setcolor preferences Select and set each parameter color and then click Save Default 2 Apply the default color scheme Click User Default to applv the color scheme The default color scheme is applied to the current file and all new files Smoothing Peaks Spectral peaks may be easier to identify by using the Smooth feature 1 From the Options menu click Smooth Spectrum To return to the display to raw data click the Smooth button on the toolbar L BEI CECENE AmE Ein Eat cose Comt Setro Yew stone Qut Somoe He lS soon A A 14 keV 6 cas samplewds lt lt gt gt lt gt Panty Panty Raw Spectral Data Smoothing Applied Labeling a Spectrum The spectral peaks represent elements in the sample Qualitative analysis measures the elements energy and relates it to elements in the periodic table The energy intensities are an indication of elements in the sample Example spectra files are available in the directory C Noran wds data Identify spectral peaks using one of the following methods Automatic IbeX MAXrav identifies peaks energy Manual You select and identify the elements 2 10 IbeX MAXrav User s Guide 136826C03 2 Using IbeX MAXrav Labeling a Spectrum Automatic This method automatically identify the element peaks in the spectrum 1 From the Options m
14. stalle zu s ubern Die Oberfl che der Diffraktoren ist empfindlich und kann sich bei Kontakt mit Reini gungsfl ssigkeiten wie Wasser aufl sen Manuelle Bedienung des Sperrventils WARNING Pumpen Sie niemals die S ule herunter wenn das Sperrventil geschlossen und das Spektrometer unter Druck ist Caution ffnen Sie niemals das Sperrventil wenn das SEM im Vakuum und das WD Spektrometer an der Luft ist Wenn man unter diesen Umst nden das Sperrventil ffnet riskiert man die Verschmutzung des Mikroskop Vakuumsystems Wenn dabei der Gl hfaden unter Strom steht kann dieser ebenso besch digt werden IbeX MAXrav User s Guide 1 11 1 Precautions and Safetv Summarv Vorsichts und Sicherheitsanweisungen WD Spektrometer Kontrolle und proportionales Z hlsystem WARNING Alle elektrischen Maschinen m ssen ber anwendbare Codes verf gen und d rfen nur von Thermo Electron Fachpersonal oder beauftragtem Fachpersonal installiert werde WARNING Im Inneren der Maschine befinden sich lebensgef hrliche Spannungen Hohe elektrische Spannungen befinden sich im inneren der Maschine Diese Spannungen k nnen schwerste Verbrennungen oder t dliche Elektroschocks ausl sen Komponenten wie Kondensatoren oder Batterien k nnen hohe Spannungen beinhalten auch wenn die Stromzufuhr unterbrochen ist Wenn Sie mit Teilen unter hohen Spannungen arbeiten m ssen Sie in jedem Fall vorher die Stromversorgung unterbrechen Entf
15. teh Bias Scan Beam Current Measure the beam current or the specimen current View Menu Modify the Labels cursor display and tool bars features in the window Cursor Display or remove the energy cursor Peak Labels Display or remove peak labels KLM Markers Display or remove the markers on the spectrum Peak Information Extract information from a peak Status Bar Display or remove the status bar located below the spectral display Toolbar Display or remove the toolbar located above the spectral display Tool Tips Display or remove the tool tips feature 3 4 IbeX MAXray User s Guide 136826003 3 Menu Reference Options Menu Vertical Arrows Displav or remove the vertical scroll buttons located on the left side of the displav These arrows are on a movable tool bar Click and drag on the space above or below the arrows to move the toolbar Horizontal Arrows Displav or remove the horizontal scroll buttons located on the bottom of the displav These arrows are on a movable toolbar Click and drag on the space to the left or right of the arrows to move the toolbar Overlav Displav or remove spectra overlavs Overlav 1 Displav or remove overlav 1 Overlav 2 Displav or remove overlav 2 Options Menu 136826C03 Preform the spectrum analvsis and modifv displav features Smooth Spectrum Displav smooth or raw spectral data Scale Spectrum Scale the spectrum to fit the displav wi
16. to the spectrum with the following procedure 1 From the View menu click KLM Markers KLM Markers Add Label Delete Label Select an element to associates with the peak Click the Table button Click once on an element to associate with the current peak and then click OK The x ray line and atomic symbol display at the peak To move through the periodic table one element at a time click the up and down arrows on the KLM Markers toolbar The current element appears in the KLM Markers toolbar If you have already applied a KLM marker to the current element in the spectrum and if the label display is turned on the marker appears on the spectrum For more information on moving to a particular region of the spectrum see Displaying a Spectrum IbeX MAXrav User s Guide 2 13 2 Using IbeX MAXrav Labeling a Spectrum Modifv the label displav e Add labels Click Add Label to display the KLM marker on the spectrum e Remove labels Click once on the element and then click Delete Label If a combination of manual and automatic labels are used and the KLM button is selected the automatic labels disappear when the Labels button is selected Remove the KLM markers window From the toolbar click the KLM Markers button Selecting Labels Create and display element labels on the spectrum 1 From the Options menu click Select Labels Select Labels Ix 7N Nitrogen E Table I Show all Kb1 l
17. 950A136826 Rev C Ibex Wavelength Dispersive Spectrometer A Xray Parallel Beam Spectrometer Thermo ELECTRON CORPORATION 2551 W Beltline Hwy Middleton WI 53562 USA Tel 800 495 3839 or 608 836 4363 Fax 608 831 4461 www thermo com IbeX MAXrav User s Guide Patents This product mav be protected bv one or more of the following US patents 5926522 Other patents may be pending Foreign patents may apply Revision history Revision Revision date Principal changes re A February 1999 Initial publication IbeX 2 0 5 B February 2000 Incorporated MAXray and Ibex WDS 3 1 0 e December 2003 Incorporates software changes WDS 3 1 6 Windows is a registered trademark of Microsoft Corporation 1999 2000 2003 Thermo Electron Corporation All rights reserved Contents Precautions and Safetv Summarv 1 1 Safetv Precautions 1 1 AG Power 1 1 P 10 Gas 1 2 IbeX MAXrav Spectrometer 1 3 Diffractors 1 4 Manual Gate Valve Option 1 4 WD Spectrometer Controller 1 5 Flow Proportional Counter Window 1 6 Motorized Retraction and Manual Retraction 1 7 SEM Venting and Window Protection 1 7 Vorsichts und Sicherheitsanweisungen 1 8 Wechselstrom Elektrizitat 1 8 P 10 Gas 1 10 IbeX MAXray Spektrometer 1 10 Diffraktoren 1 11 Manuelle Bedienung des Sperrventils 1 11 WD Spektrometer Kontrolle und proportionales Z hlsystem 1 12 Das Fenster des Zahlers der den proportionalen Flu misst 1 13 Manuelles o
18. AGE system Select Mixed or User for the type of references in the periodic table Quant Parameters window Make sure the correct References Database is selected in the window In the SPA dialog menu select Acquire Options Concurrent WDS and define whether the count of the WDS is to be conducted before during or after the EDS count IbeX MAXrav User s Guide 2 45 2 Using IbeX MAXrav Exiting IbeX MAXray 3 Make sure the beam current and keV are correct in the VANTAGE column tool and start the combined EDS WDS acquisition by clicking the start icon in the spectral display QuickClick bar The beam current for tne WDS count will be obtained from tne BANTAGE column tool The files in the wds_standards directory will be scanned for the fie that has the correct keV and correct WDS elements for the count If more than one file satisfies these criteria the operator will be prompted to select the correct file 4 When the count is complete the Quantitative Analysis icon on the QuickClick bar of the spectral display window can be used to obtain the quantitative results for the sample Exiting IbeX MAXrav To exit the IbeX MAXrav program use one of the following procedures From the File menu click Exit e Hold down Alt on the keyboard and then press F4 e Click the Close button X in the top right corner of the main window 2 46 IbeX MAXrav User s Guide 136826C03 3 Menu Reference Each menu contains options for preforming operat
19. Acquire Peak to Background Acquire Peak To Background Procedure Peak BkgdLo Bkgd Hi Time Gross Bkad Peak To Element Line Diffractor kev keV kev sec Counts Counts Background Si Kal PET 1 740 1 621 1 878 7330 13 548 257 A 0 Kat WSi60 0 523 0 469 0 591 10 23465 615 38 125 r Procedure r Edit Data Acquisition f Edit Insert Start Stop Save P B Print Delete Continue Pause Acquire One Close Ready 136826003 IbeX MAXrav User s Guide 2 39 2 Using IbeX MAXrav 2 Insert elements Click Insert and then click Table to select an element Table Element 14Si X rayLine Kal Diffractor PET h Peak kev 1 740 Bkgd Lo ke 1 621 Bkgd Hi kev 1 878 Acquisition Time sec Peak Search Parameters Begin End Ste Dwell 1 728 key 1 752 key 2 eV 1 Bee care Quantitative Analvsis Select an element by clicking the Table button The following fields display Verifv and change information if needed X ray Line K L or M line Diffractor The diffractor Peak The peak centroid location 3 Select the Peak Search Parameters Bkgd Lo The location of the low energy background count Bkgd Hi The location of the high energy background count Peak Search Select this check box to preform a peak search Acquisition Time The amount of time to obtain the peak centroid counts Both options can be sele
20. EDS WDS Analvsis 9 Print the report Click OK The spectrum prints Procedure for Combined EDS WDS Analvsis The optional WDS interface equipment is required to preform the following analysis 136826C03 Qualitative Analvsis 1 In the VANTAGE EDS spectral display define a region of interest ROI covering the energy range desired for a WDS scan Place the cursor within the defined ROI Click the WDS icon on the spectral display QuickClick bar to start the wavelength scan When the scan is complete the WDS scan will be placed in a spectral area on the VANTAGE system and the EDS spectrum will be overlapped with th e WDS scan in the spectral display window Quantitative Analysis Setting Up Standards Standards must be used to obtain k ratios for all elements whose weight concentrations are to be measured in the sample 1 Count standards for the WDS elements on the MAXrav or IbeX spectrometer at the same conditions as will be used for the sample and save the standards file in the directorv named wds standards Count standards for the EDS elements on the VANTAGE svstem Make sure the beam current is correct in the VANTAGE column tool when the EDS acquisitions are started Store references obtained from the EDS spectra by using the References option under the Tools menu on the spectral display window Sample Count 1 Define the elements to be analyzed with EDS and WDS in the quantitative periodic table on the VANT
21. MAXrav 2 Editelements Click Edit and then click Table to select the element Table Element 145i x ray Line Kal Diffractor PET Peak keV 1 740 BkgdLo keV 1 621 Bkgdhi kev fs O Standard sina Standard Time sec 60 UnknownTime sec B Beam Current nAmps ooo oo Area Peak Factor foo Peak Search M OnStd Peak Search Parameters Begin End Step Dwell 1 728 ke 1 752 keV 2 jew 1 ec care Quantitative Analvsis The following fields displav Select the Standard element from the drop down list and verifv the remaining fields X ray Line K L or M line Diffractor The diffractor 3 Select the Peak Search Parameters Peak The peak centroid location Bkgd 1 The low background count location Bkgd 2 The high background count location Standard The standards element defined during element setup Standard Time The amount of time to acquire the Standard Beam Current The beam current acquiring standards Unknown Time The amount of time to acquire the unknown element Area Peak Factor Adjust for changes in a peaks shape in carbon analysis Both options can be selected Any edits you make in this area display in the Peak Search 2 36 IbeX MAXray User s Guide 136826C03 2 Using IbeX MAXrav Quantitative Analvsis dialog box For more information see Peak Search Select On Std to preform a peak search on the elem
22. Parameters Edit the data acquisition conditions Acquire Menu Collect the spectral data from the spectrometer Element Scan Quickiv scans an element or defined energv range 3 2 IbeX MAXrav User s Guide 136826C03 3 Menu Reference Count Menu Setup Scan Set or view the scan parameter Peak Search Locate the centroid of a peak Start Scan Begin the scan procedure Scan Setup must be completed prior to starting the scan Stop Scan Stop a scan already in progress Pause Scan Pause a scan already in progress For example pause a long scan to check the beam position spot mode Click Continue to resume the scan Count Menu View the rate meter and x ray counts Rate Meter Display an analog rate meter Counter During acquisition display the total number of counts elapsed time and count rate Settings Menu 136826003 Modify and view information about diffractors or position the spectrometer Configuration Display the available diffractors and energy ranges Position Spectrometer Position the diffractor or detector to the correct Bragg angle IbeX MAXrav User s Guide 3 3 3 Menu Reference View Menu Bias Scan Determine the detectors bias voltage to fine tune the detector voltage This option is used with the SCA Scan SCA Scan Determine the x ray lines single channel analyzer voltages fine tune the detector bias voltage found with the bias scan function This option is used with
23. Precautions 1 1 1 2 1 4 1 5 1 6 1 7 Index Previewing a Report 3 2 Printer Resolution 2 43 Printing 2 16 Options 3 2 Peak to Background Information 2 41 Preview a Report 3 2 Reports 2 43 3 2 Standard Information 2 37 Standards 2 34 Proportional Counting System 1 5 Proza PRZ 2 38 Q Quant Analysis 2 25 Menu 3 6 Quantifiable Peaks 2 39 Quantitative Analysis 2 30 2 34 R Rate Meter 2 27 3 3 Recording Acquisition Information 3 2 Relative Intensity 2 15 Report Printing 2 16 Reports 2 43 Resetting the Motors 3 7 Results 2 38 3 7 S Safety Summary 1 1 Sample 2 16 Set Up 2 15 Saving A Peak to Background File 2 41 A Standards File 2 34 Acquisition Setup 2 23 EMSA File 3 2 Files 3 1 Spectrum 2 29 Unknowns File 2 37 Index 3 Index SCA Baseline 2 21 2 23 Scan 2 18 3 4 Window 2 21 2 23 Scaling A Spectrum 2 7 3 5 An Overlay 3 5 Scan Energy Range 3 2 Parameters 3 2 Setup 3 3 Scanning for One Element 2 19 Scroll Bars 2 3 Scrolling 2 7 3 5 Searching fora Peak 3 3 Select Labels 3 6 Selecting Labels 2 14 SEM Venting 1 7 Service Menu 3 7 Setting Up Acquisition Information 2 16 Acquisitions 2 15 Elements 2 30 Microscope 2 15 Printer Resolution 2 43 Samples 2 15 Scan Parameters 2 20 3 2 Standards 2 30 3 6 Settings Menu 3 3 Shifting Peaks 2 26 Shortcuts 3 4 Single Channel Analyzer Scan 2 18 3 4 Smooth 2 26 2 27 Smoothing Peaks 2 10 2 29 Spectrum 2 29 3 5 Software controls
24. Set Up Up to 6 acquisition setup procedures can be stored using the User Scan buttons Apply the saved setup by clicking on the User Scan buttons la 136826C03 Define the element parameters to save Set the parameters to associate with a User Scan button For more information see Setting Up The Scan Parameters IbeX MAXrav User s Guide 2 23 2 Using IbeX MAXrav Save the setup Click a User Scan butt Scan Parameters on Restore All Restore Be Save Be Dan ja Table User Scan 1 User Scan 3 User Scan 5 User Scan 2 User Scan 4 User Scan 6 Peak Energy Scan le x Ihe ae al Beginning Energy 0 000 key Paak Search Ending Energy 0 000 keV X ray Line Step Size p a v Dwell Time 0 0 sec Diffractor Detector C c Bias f volts C C SCA Baseline 0 00 volts C C SCA Window 0 00 volts Enter aname for the parameters set Scan Name Ix Enter a name for this scan button Setting Up a Scan Acquisition User Scan Buttons Tvpe a name for the set a maximum of nine character and then click OK The name displavs on the button 2 24 IbeX MAXrav User s Guide 136826C03 2 Using IbeX MAXrav Setting Up a Scan Acquisition Beam Current An accurate beam current must be obtained for Quant Analysis Current varies for many reason at acquisition time Not all systems have the optional equipment necessary to preform this procedure 1 From the Settings
25. The selected check boxes determine the report information that prints Verifv the information and then click Close to applv the changes 7 Print the report From the File menu click Print The print dialog box displays Select a printer from the Name drop down list Print Printer Name Status Ready Type HP LaserJet 4000 Series PS Where 132 9 200 106 Comment Properties 7 Print to file r Print range Copies All Number of copies fi a Pages from 1 tof A Cancel 8 Change the printer resolution Click the Properties button The selected printers properties dialog box displays Select the Advanced tab 6 Manufacturing HP 4000 Document Properties Page Setup Advanced EA HP LaserJet 4000 Series PS Document Settings EA Paper Dutput Paper Size lt Letter gt A Orientation lt Portrait gt BI Paper Source lt Automatically Select gt A Copy Count lt 1 Copy gt FIR Print on Both Sides Duplex Printing lt Long Side gt In Graphic EE Resolution lt 300 gt E Color Appearance lt Gray Scale gt R Scaling lt 100 gt r Change Resolution Setting Under Graphics click once on Resolution The resolution options display at the bottom of the dialog box change resolution settings Click once on 300 and then click OK 2 44 IbeX MAXrav User s Guide 136826C03 2 Using IbeX MAXrav Procedure for Combined
26. Xrav User s Guide 2 21 2 Using IbeX MAXrav 4 Select acquisition parameters for individual elements Setting Up a Scan Acquisition Click the Parameters button For more information see Saving the Acquisition Set Up Scan Parameters Ix 4 Be Berlium E Table User Scan 1 User Scan 3 User Scan 5 User Scan 2 User Scan 4 User Scan 6 Peak Energy Scan a Thesretical Beginning Energy 0 000 keV 0000 kev L Se rasen Ending Energy 0 000 kev KNE Step Size ev v Dwell Time p i sec Diffractor Detector c c Bias p volts c C SCA Baseline 0 00 volts C C SCA Window fi 00 volts Restore All Restore Be Save 5 Select an element Click the up and down arrows to select an element or click Table to select from a periodic table of elements 6 Select the Peak Energy option The selected energy keV displays when a select is made Select Theoretical to use the determined energy value Select Peak Search to use the energy value determined during the peak search For more information see Peak Search 7 Select the X ray lines Click the X ray Lines drop down box to select the K L M and N lines of interest 8 Select a diffractor Diffractor settings are passed to the Scan Setup Window The diffractor options may vary from spectrometer to spectrometer 9 Enter the elements scan parameters Beginning Energy The scans minimum energy level in keV Ending Energy
27. actor Counts Counts n mp k ratio Weight Weight WSi6D 153338 154734 236 392 0 3272 53 77 0 19 Si K PET 44036 44204 67 888 0 4169 47 03 0 32 Total 100 80 Accelerating Voltage 4 p Specimen Tilt Angle Correction Model ccelerating Voltage pecimen Tilt Angle orrection Mode GF Standards 0 deg de CP 00 ku time ae Print Sample Odeg deg C ZAF Show Formula 2 Apply a matrix Correction Mode Proza A PRZ correction routine modified by Thermo Electron e ZAF Account for Atomic number Z Absorption A and Fluorescence F 3 View or change the Stoichiometric formula Click Show Formula Define One Element in the Formula EA Basis Element Number of Atoms Cancel Select an element from the Basis Element drop down list Change the number of atoms Click OK to save the changes and exit Click Cancel to exit without saving changes 4 Save the results file The atomic percent for the defined element displays in the result window and the calculated atomic percent for the remaining unknown elements Click Save type the results file name the file extension rit is automatically added 2 38 IbeX MAXray User s Guide 136826C03 2 Using IbeX MAXrav Quantitative Analvsis 5 Exit Results Click Close Acquire Peak to Background The Peak to Background acauisition determines if there is a detectable and quantifiable peak 1 From the Quant menu click
28. acuum of the spectrometer and the SEM chambers is made of polypropylene If the window must be replaced follow these precautions Caution Shut off the high voltage to the detector Caution Turn off the P 10 gas Caution Solvents must not come into contact with the window 1 6 IbeX MAXrav User s Guide 136826C03 1 Precautions and Safety Summary Safety Precautions 136826003 WARNING Do not seal off the gas flow routinely or the window will break Motorized Retraction and Manual Retraction Do not change the retraction limits set during installation SEM Venting and Window Protection Always loosen an unused port cover before venting the SEM Air or nitrogen entering the chamber can easily break the proportional counter window IbeX MAXrav User s Guide 1 7 1 Precautions and Safetv Summarv Vorsichts und Sicherheitsanweisungen Vorsichts und Sicherheitsanweisungen Aufschriften und Dokumente f r den IbeX MAXray unterteilten Vorsichts ma nahmen in WARNUNG und VORSICHT WARNUNG wird gebraucht wenn eine gef hrliche oder unsichere Benutzung in schwersten oder t dlichen Verletzungen enden kann VORSICHT wird gebraucht wenn eine gef hrliche oder unsichere Benutzung in geringeren Verletzungen oder Sachbesch digung enden kann Andere Empfehlungen f r den Gebrauch des Produkts werden mit WICHTIG oder NOTIZ angef hrt Ihre Thermo Electron Maschinen sind entworfen und getestet um den strengsten Sicherheitsanforde
29. ation to print on the results report Select the check boxes to include on the results report For more information see Printing Reports 4 Apply the changes to Acquisition Information e Click Close e Click Clear to delete all Acquisition Information Bias Scan Determine the detectors bias voltage for an x ray line 1 2 Focus the microscope on the element of interest and then position the spectrometer From the Settings menu click Bias Scan Stat V 1800 End V 2300 Step V jo Dwell sec fo Correct Bias Voltage Start Stop 1800 1900 2000 2100 2200 2300 s Begin the Scan Use the systems default settings Click Start Center the correct bias voltage IbeX MAXrav User s Guide 2 17 2 Using IbeX MAXrav Setting Up a Scan Acquisition The correct bias voltage is above the first shoulder and prior to the sharp peak If this point is not visible or not centered on the display modify the starting voltage until the correct voltage is determined The example above shows a centered voltage point e If the display is to far left Increase the starting bias and decrease the ending bias by the same amounts e If the display is to far right Decrease the starting bias and increase the ending bias by the same amount 5 Exit Bias Scan Click Close SCA Scan A single channel analyzer SCA scan fine tunes the detector bias voltage found with the Bias Scan function The Detector
30. brauchen Sie eine T 250V 3A Sicherung e F r 230 240 VAC Betrieb brauchen Sie zwei T 250V 2A Sicherungen 5x20 mm Caution Um einen dauernden Feuerschutz zu gew hrleisten wechseln Sie die Sicherung nur mit den genannten Typen aus Caution Legen oder stellen Sie niemals Objekte irgendwelcher Art die eine K hlung ver meiden k nnten unter oder um den Boden der Kontrolle Never operate your Thermo Electron equipment if you notice unusual noises or foul odors Disconnect the power cord from the main power source and call your Thermo Electron support specialist Das Fenster des Z hlers der den proportionalen Flu misst Das Material das das Gas im Inneren der Anzeige vom Vakuum des Spektrometers und der SEM Kammern isoliert ist aus Polypropylen gemacht Falls Sie das Fenster ersetzen m ssen halten Sie sich an diese Sicherheitsanweisungen Caution Unterbrechen Sie die Stromzufuhr der Anzeige Caution Drehen Sie das P 10 Gas ab Caution Keine L sungsmittel d rfen mit dem Fenster in Ber hrung kommen 136826C03 IbeX MAXrav User s Guide 1 13 1 Precautions and Safetv Summarv Vorsichts und Sicherheitsanweisungen WARNING Dichten Sie den Gasflu nicht mechanisch ab oder das Fenster bricht Manuelles oder motorgetriebenes Zur ckziehen Nehmen Sie keine nderungen an den bei der Installation eingestellten R ckzugs begrenzungen vor SEM L ftung und Schutz des Fensters ffnen Sie stets einen unbenut
31. connect Thermo Electron equipment to a power source receptacle that lacks ground connection terminals Never operate your Thermo Electron equipment if you notice unusual noises or foul odors Disconnect the power cord from the main power source and call your local Thermo Electron support specialist WARNING Avoid contact with internal high voltage sources Never remove any outer covers or guards that are fastened with screws without being so instructed either by this manual or by a qualified Thermo Electron support specialist Never attempt internal service or system adjustments unless instructed to do so either by this manual or by a qualified Thermo Electron support specialist Never remove system connections when power is applied Never override or cheat electrical or mechanical interlock devices When working around high voltage sources be sure all power inputs are disconnected When working around capacitors batteries and other power sources allow a few minutes for capacitors to discharge after power has been removed Avoid contact direct or through metal tools or jewelry with any uninsulated internal electrical component without being so instructed either by this manual or by a qualified Thermo Electron support specialist Caution The fuse in the power entry module must match the line voltage P 10 Gas The flow proportional counter requires a special gas called P 10 Tanks of P 10 gas are available
32. cted Any edits you make in this area display in the Peak Search dialog box For more information see Peak Search Select On Std to preform a peak search on the element at the designated energy val ues e Select on Unk to preform a peak search on the unknown element at the designated 2 40 IbeX MAXrav User s Guide 136826C03 2 Using IbeX MAXrav Quantitative Analvsis 136826C03 energy value 4 Begin the acquisition Click Start to acquire all elements The following prompts displav to verifv set up information Acceleration Voltage Position beam on Standard e Insert the Faraday Cup Enter the Beam Current e Remove the Faraday Cup The acquisition begins The status of the acquisition displays at the bottom of the IbeX MAXrav window The acquisition stops automatically e Click Pause to temporarily stop the acquisition Click Start to acquire all elements starting at the beginning of the list e Click Acquire One to start and stop after acquiring the currently selected highlighted element Click Continue to acquire element in the list starting at the currently selected high lighted element and continue through the list in the order they appear e Click Stop to end the acquisition prior to the designated acquisition time 5 Save the Peak to Background file e Click Save P B Enter the file name and then click OK e Click Load P B to re acquire a previously saved file Click
33. der motorgetriebenes Zur ckziehen 1 14 SEM Liftung und Schutz des Fensters 1 14 Using IbeX MAXrav 2 1 Software Controls and Layout 2 1 Menu Bar 2 1 Toolbar 2 1 Microsoft Windows NT Tools 2 2 Active Window 2 2 Click and Drag 2 2 Scroll Bar 2 3 Drop Down Box 2 3 Check Boxes 2 4 Option Buttons 2 4 Text Fields 2 5 Starting IbeX MAXrav 2 5 Initializing the System 2 6 Opening Files 2 6 Contents Displaving a Spectrum 2 7 Displav Options 2 8 Changing Displav Colors 2 9 Customizing the Default Color Scheme 2 10 Smoothing Peaks 2 10 Labeling a Spectrum 2 10 Automatic 2 11 Manual 2 11 Peak Hints 2 11 Peak Information 2 12 Displaving KLM Markers 2 13 Selecting Labels 2 14 Setting Up a Scan Acquisition 2 15 Microscope and Sample 2 15 Acauisition Information 2 16 Bias Scan 2 17 SCA Scan 2 18 Scanning for One Element 2 19 Scan Parameters 2 20 Saving the Acquisition Set Up 2 23 Beam Current 2 25 Peak Search 2 26 Rate Meter 2 27 Counter 2 28 Acquiring a Spectrum 2 28 Saving a Spectrum 2 29 Quantitative Analysis 2 30 Setup Standards 2 30 Acquire Standards 2 31 Acquire Unknowns 2 34 Results 2 38 Acquire Peak to Background 2 39 Matrix Correction and Linear Regression 2 41 Printing Reports 2 43 Procedure for Combined EDS WDS Analysis 2 45 Qualitative Analysis 2 45 Quantitative Analysis 2 45 Setting Up Standards 2 45 Sample Count 2 45 Exiting IbeX MAXray 2 46 Contents Menu Reference 3 1 File Menu 3 1
34. duce to an icon Exit the File Edit Acquire Count Settings View Options Quant Service Help Program keV cts Active Window Multiple windows can be displayed at the same time However only one window accepts commands This windows is referred to as the active window To activate a window click once on the window to activate You can tell a window is active when the title bar is dark blue or the customized Microsoft Windows setting Inactive windows are grey Click and Drag Most commands are preformed by clicking or double clicking with your mouse Clicking and dragging involves moving or positioning am object For example moving a window to a new location on the desktop To click and drag an object left click on an item hold down the mouse button and then move the object to the desired location Use the click and drag technique to Shift the spectrum left or right by clicking and dragging with the right mouse button lbeX MAXray User s Guide 136826C03 2 Using IbeX MAXrav Software Controls and Lavout 136826C03 Shift the spectrums vertical scale by clicking and dragging with the right mouse button up or down Hold down both mouse buttons and drag left or right to scale shrink or expand the spectrum Scroll Bar A scroll bar moves the display up down left or right To scroll quickly click and drag the slider Click the scroll bar arrow to move slowiv Scroll Arrow
35. e of minutes e Click OK to initialize Click Cancel to exit without initializing Opening Files IbeX MAXray displays wds wdx or EMSA files Files with the extension EMSA are accessed with the Open EMSA option in the File menu Open wds and wdx files with the following procedure 1 From the File menu click Open Look in J data cl Fie name Files of type WDS Spectrum Files wdx bel Cancel I Open as read only 1 Select a file name Double click on the file name to display or change directories by clicking the Look In drop down arrow Thermo Electron provides example files in the directory C Noran wds data 2 Open the file Click Open to display the file 2 6 IbeX MAXray User s Guide 136826C03 2 Using IbeX MAXrav Displaving a Spectrum Click Cancel to exit without opening a file Displaying a Spectrum Several display options are available for viewing the spectrum The diagram below labels the location of each control Remove Element Labels im NORAN Ibex File Edit Acquire Count Settings View Options Quant Service Help Open Save Smooth Seale KIM identity Labels scan Stop Peak Energy 740 keV 3284 cts W_Si wdx and Counts Change Vertical Scaling Expand or Contract Expand the spectrum Click the lt and gt button Contract the spectrum Click the gt and lt button Scroll left and right
36. eX MAXray User s Guide 2 Using IbeX MAXrav Printing Reports Printing Reports Print the spectrum and associated acquisition information in a formatted report For best results set vour prints resolution to 300 dpi the procedure for setting vour printers resolution is described below 1 136826003 Display the spectrum Verify the current display contains the labels and colors you want on the report For more information see Displaying a Spectrum From the File menu click Print Options Spectrum Acquisition Parameters Printer Margins Line Al Left fo Filled Selection Color C None Top j100 J OK Cancel Select print options Select the spectrum parameters e Line Print the spectrum as an outline Filled Print the spectrum as a histogram Color Print the spectrum in color histogram Select the acquisition parameters e All Print all acquisition parameters Selection Print selected acquisition parameters selections are made later in this pro cedure None Print the spectrum only Enter the Left and Top margins in pixel 100 pixels is approximately 1 inch Save the Print Options Click OK to save the changes and exit e Click Cancel to exit without saving the changes Verify the Acquisition Information IbeX MAXrav User s Guide 2 43 2 Using IbeX MAXrav Printing Reports From the Edit menu click Acquisition Information
37. emals Maschinen von Thermo Electron an nicht korrekt geerdete Steckdosen an e Arbeiten Sie niemals mit Maschinen von Thermo Electron wenn Sie beim Betrieb merkw rdige Ger usche oder Ger che wahrnehmen Unterbrechen Sie die Stromversorgung und rufen Sie ihren rtliche Thermo Electron Fachmann an Vermeiden Sie jeden Kontakt mit Maschinenteilen unter Hochstrom Entfernen Sie keine Abdeckungen oder Schutzbleche die mit Schrauben befestigt sind wenn Sie nicht durch diese Anweisung oder einen Spezialisten von Thermo Electron dazu aufgefordert werden Versuchen Sie niemals Einstellungen oder Reperaturen an den Maschinen zu machen wenn Sie nicht durch diese Anweisung oder einen Spezialisten von Thermo Electron dazu aufgefordert werden Entfernen Sie keine Verbindungen zwischen den Systemen wenn die Maschine unter Strom steht Schlie en Sie niemals elektrische oder mechanische Unterbrechungen kurz Wenn Sie mit Teilen unter hohen Spannungen arbeiten m ssen Sie in jedem Fall vorher die Stromversorgung unterbrechen Wenn Sie in der N he von Kondensatoren Batterien oder anderen Quellen von Elektrizit t arbeiten warten Sie nach der Unterbrechung des Stromkreises einige Minuten damit sich die Restspannung entladen kann Vermeiden Sie jeden Kontakt direkt oder durch Metallwerkzeuge oder Metallschmuck mit inneren nicht isolierten Maschinen teilen wenn Sie nicht durch diese Anweisung oder einen Spezialisten von Thermo Elect
38. ements B C N O and F by stoichiometry In this case define a chemical formula for each element in the acquisition list to provide the necessary stoichiometric relationships 2 34 IbeX MAXrav User s Guide 136826003 2 Using IbeX MAXrav Quantitative Analvsis 1 From the Quant menu click Acquire Unknowns Procedure Quartz std Analysis Type Matrix Correction Beam 100 kv Tit deg Azimuth deg Peak BkadLo BkadHi Time Beam Unknown Count Element Line Diffractor kev keV kev Standard sec nAmp Counts Error 0 Kat WSIBD 0 523 0 469 0 591 oxygen 60 10 811 153338 391 E Si Kal PET 1 740 1 621 1 878 silicon 60 10 811 44036 209 Procedure r Edit Data Acquisition Load Unk Load Std Edit T Start Stop Save Unk Print Delete Prijur Continue Pause Define wi l EDS K Ratio Acquire One Results Close If analyzing a set of elements for the first time click Load Unk Edit an element by clicking once on the element to modify and then click Edit Delete an element by clicking once on the element to remove and then click Delete Modify the Weight percent by clicking once on the element to modify and then click Define Wt Enter a K Ratio by clicking once on the element to modify and then click EDS K Ratio Modify the Stoichiometry by selecting from the Stoichiometry drop down list and then click Change 136826003 IbeX MAXrav User s Guide 2 35 2 Using IbeX
39. ent at the designated energy val ues Select on Unk to preform a peak search on the unknown element at the designated energy value 4 Begin acquiring unknowns elements Click Start to acquire the unknowns elements or click Acquire One to acquire data for the currently selected element only The following prompts display to verify set up information Acceleration Voltage Position beam on Standard e Insert the Faraday Cup Enter the Beam Current e Remove the Faraday Cup The acquisition begins The status of the acquisition displays at the bottom of the IbeX MAXrav window The Acquisition stops automatically e Click Pause to temporarily stop the acquisition Click Continue to start the acquisition where it was stopped e Click Stop to end the acquisition prior the designated acquisition time 5 Save the acquisition Click Results to view the acquired information For more information see Results e Click Save Unk Enter a file name and then click OK Click Print to print the currently displayed element information Click Close to exit Acquire Unknowns 136826C03 IbeX MAXrav User s Guide 2 37 2 Using IbeX MAXrav Quantitative Analvsis Results Select the matrix correction method for calculating each elements weight percentages in the sample 1 From the Quant menu click Results Results Standards Procedure Quartz std Peak Standard Cps Element Error Element Line Diffr
40. ents the x ray counts at each energy level peak intensity Stop the acquisition Click the Stop button or wait until the acquisition ends automatically lbeX MAXray informs 2 28 IbeX MAXrav User s Guide 136826003 2 Using IbeX MAXrav Acquiring a Spectrum you when the acquisition is finished Click OK to continue You cannot resume an acquisition after clicking Stop 3 Display the spectrum with smooth peaks Click the Smooth button Saving a Spectrum Periodically save files by selecting the File menu and the click Save To save a file for the first time or to save in a new directory use the following procedure 1 From the File menu click Save As Save a WDS Spectrum File 27x Save in J data cH Save as type WDS Spectrum Files wds sl Cancel I Open as read only 2 Enter a file name Type a file name in the File Name text box field The file extension WDX is automatically added to the file name 3 Select a directory location Click the Save In drop down list to select a file location DO NOT store files in the directory C Noran wds data To prevent deleting files it is a good practice to save files in a user defined directory 4 Save the file Click OK 136826C03 IbeX MAXrav User s Guide 2 29 2 Using IbeX MAXrav Quantitative Analvsis Quantitative Analvsis At least one standard must be defined for each element in the unknown sample Quantitative analvsis calculates t
41. enu Click Identify Peaks Labels display for each element and x ray line name Peaks are labeled by the atomic symbol and x ray line name li NORAN IbeX Biel Eg File Edit Acquire Count Settings View Options Quant Service Help Open Save Smooth Scale KLM identity scan Start Stop A W_Si wdx 2 Remove the displayed labels Click the Labels button on the toolbar Manual To identify peaks manually some knowledge of spectral microanalysis is necessary For more information read Scanning Electron Microscopy and X Ray Microanalysis A Text for Biologists Materials Scientists and Geologists 2nd ed by Joseph I Goldstein et al Chapters 6 8 Peak Hints For assistance in identifying peaks use the Peak Hints option 1 From the Options menu click Peak Hints The dialog boxes left side displays peaks to the left of the cursor position The dialog boxes right side displays peaks to the right of the current cursor position 136826C03 IbeX MAXrav User s Guide 2 11 2 Using IbeX MAXrav Labeling a Spectrum To change the display labels move the cursor over the spectrum Each peak is identified by the atomic symbol x ray line name relative intensity 1000 highest probabilitv of the peak existing and energy in keV Sb M503 10 0 525 Delete Label Threshold Close 2 Modify Peak Hints Add labels Click once on an element and then click Add Label Remove labels
42. ernen Sie keine Abdeckungen oder Schutzbleche die mit Schrauben befestigt sind wenn Sie nicht durch diese Anweisung oder einen Spezialisten von Thermo Electron dazu aufgefordert werden Versuchen Sie niemals Einstellungen oder Reperaturen an den Maschinen zu machen wenn Sie nicht durch diese Anweisung oder einen Spezialisten von Thermo Electron dazu aufgefordert werden Sorgen Sie daf r da die Maschinen korrekt geerdet sind Schlie en Sie die Maschinen nur an korrekt geerdete Steckdosen an Wenn Sie unsicher sind lassen Sie die Steckdose von einem Fachmann untersuchen Schlie en sie niemals Maschinen von Thermo Electron an nicht korrekt geerdete Steckdosen an Caution Die Kontrolle mu gem den Vorschriften installiert werden wie sie in der Mon tageanleitung und in der Betriebsanweisung vorgeschrieben werden um das Spektrometer nicht zu besch digen Caution Die Sicherung die Sicherungen in der Kontrolle m ssen der allgemeinen Span nung entsprechen 1 12 IbeX MAXrav User s Guide 136826003 1 Precautions and Safetv Summarv Vorsichts und Sicherheitsanweisungen Caution Pr fen Sie nach da die Sicherungen f r den Wechselstrom korrekt sind Das Wechselstromaggregat hat einen universellen Mechanismus der es berfl ssig macht Kabel oder Schalter anzubringen um die Maschine den verschiedenen Stromspannungen anzupassen Die Sicherung mu dennoch korrekt installiert sein e F r 100 120 VAC Betrieb
43. es 2 29 Text 2 5 Exiting the Program 2 46 3 2 Extract Information 3 4 F File Extension 2 29 Menu 3 1 Name 2 16 2 29 Types 2 6 Flow Proportional Counter Window 1 6 G Graphing 2 28 Index 2 IbeX MAXrav User sGuide H Help Identifing Peaks 2 11 Help Menu 3 7 Hints 3 6 Horizontal Scroll 3 5 How To 3 8 I Icons 3 4 Identification 2 16 Identify Peaks 2 11 Peaks Elements 2 10 2 39 3 6 Initializing Motors 3 7 The System 2 6 Instrument Set Up 3 2 K KLM Markers 2 13 3 4 L Labeling a Spectrum 2 10 Labeling Peaks 3 6 Loading A Peak to Background File 2 41 A Standards File 2 34 Standards 2 35 Look In 2 6 Low Level Discriminator LLD 2 18 M Magnification 2 17 Manual Gate Valve Option 1 4 Peak Identification 2 11 Retraction 1 7 Matrix Correction Mode 2 38 IbeX MAXrav User sGuide Menus 2 1 Microscope model 2 17 Microscope Set Up 2 15 Microsoft Windows Tools 2 2 Modifing Colors 3 6 Display 3 6 Motorized Retraction 1 7 N Navigating 3 7 Number of Atoms 2 30 O Offset an Overlay 3 5 One Element Scanning for 2 19 Opening EMSA Files 3 2 Files 2 6 3 1 Option Buttons 2 4 Options Menu 3 5 Overlays 2 9 3 1 Viewing 3 5 P P 10 Gas 1 2 Pausing a Scan 3 3 Peak Analysis 2 10 Hints 2 11 3 6 Identification 2 11 Information 3 4 Labels 3 4 3 6 Search 2 26 3 3 Shift 2 26 Smoothing 2 10 to Background 3 7 Peak Labels 2 10 Positioning the Spectrometer 3 3
44. from local bottled gas suppliers The tank of P 10 should have a two stage regulator with a 1 4 NPT fitting to accept the Thermo Electron supplied third stage regulator IbeX MAXrav User s Guide 136826C03 1 Precautions and Safety Summary Safety Precautions 136826003 WARNING P 10 gas is a HAZARDOUS MATERIAL Handle P 10 gas in accordance with the manufacturer s Material Safety Data Sheet WARNING Fasten the tank of P 10 gas securely to a fixed object such as a wall or workbench to avoid damage to the tank The tank contains hazardous material under pressure The tank is dangerous if its valve is damaged or the tank is punctured However the gas is not flammable IbeX MAXrav Spectrometer Caution Be sure the spectrometer working distance is correct WD spectrometers are designed to be used at a specific working distance from the sample Consult your microscope manual for the recommended working distance for your equipment Caution Caution Caution Caution Caution Caution A high voltage cable connects the PCS box to the WD spectrometer Do not dis connect this cable unless the entire system is powered off Setting the bias voltage for the detector too high could shorten the life of the detector Use the bias scan to determine the proper voltage Initialize the spectrometer properly to avoid moving it beyond a hard limit The IbeX MAXrav spectrometer should not come into contact with any
45. he concentration of elements in the sample The calculated concentrations are based on a net peak intensities of a standard and the unknown elements A PROZA or ZAF matrix correction compensates for the mix of concentrations of elements Setup Standards Define the elements that will be used in the standards file The elements are defined bv weight percent or the number of atoms stoichiometrv 1 From the Quant menu click Setup Standards Standard Name BUEME F Stoichiometry Add Delete Clear All Element Weight Find Save Close 2 Enter the Standards Name Type a name in the Standard Name text box maximum of ten characters To locate a previously saved Standard file click Find A list of Standards files displays Click once on the file name to display and then click Select 3 Select how to define elements Elements are defined by a weight percent of the total standard or by number of atoms in the standard Select Stoichometry to define elements by atoms When the Stoichiometry check box is not checked the elements are setup by number of atoms 4 Define the elements in the standard 2 30 IbeX MAXrav User s Guide 136826C03 2 Using IbeX MAXrav Quantitative Analvsis e Click Add The Add Element to Standard dialog box displays Select element 5B Enter Weight Percent OK Cancel Click Table to select an element enter number of atoms or the weight percent and then click OK
46. he filament is powered on it may also be damaged 1 4 IbeX MAXrav User s Guide 136826003 1 Precautions and Safety Summary Safety Precautions 136826003 WD Spectrometer Controller WARNING All electrical equipment must meet applicable codes and must be installed by Thermo Electron authorized support representatives WARNING Dangerous voltages are present inside the equipment High operating voltages are present inside the equipment These voltages can produce burns or fatal electrical shocks Numerous internal components operate at high voltages and may not be insulated or shielded Components such as capacitors can store high voltages even with the power disconnected When you are working around high voltage sources be sure all power inputs are disconnected Never remove any outer covers or guards that are fastened with screws without being instructed by this manual or by a qualified Thermo Electron support specialist Never attempt internal service or system adjustments unless instructed to do so either by this manual or by a qualified Thermo Electron support specialist Maintain proper equipment grounding Always connect equipment to a properly grounded power source receptacle If in doubt have the receptacle checked by a qualified technician Never use a ground adapter plug to connect Thermo Electron equipment to a power source receptacle that lacks ground connection terminals Caution Do not move the stage when
47. icht wenn zuvor nicht die Stromzufuhr unterbrochen ist Caution Wenn die Vorspannung f r die Anzeige zu hoch eingestellt wird kann die Leb ensdauer der Anzeige verk rzt werden Caution Das Spektrometer mu sorgf ltig eingearbeitet werden damit es sich nicht auf zu hohe Limits zubewegt Caution Das IbeX MAXrav Spektrometer sollte nicht mit Zubeh r in Kontakt kommen das nicht von Thermo Electron ist 1 10 IbeX MAXray User s Guide 136826003 1 Precautions and Safetv Summarv Vorsichts und Sicherheitsanweisungen 136826C03 Caution Ber hren Sie das Fenster des Diffraktors oder des Z hlers der den Durchflu misst nicht anders als in den Installationsanweisungen vorgeschrieben Caution Ber hren Sie nicht die inneren Teile des Spektrometers mit ihren H nden oder l von der Oberfl che ihrer H nde k nnte das Spektrometer verunreinigen und die Abflu zeit verl ngern Caution Verkratzen Sie nicht die O Ringe der aufeinanderarbeitenden Oberfl chen oder die Flange an den Schnittstellen Caution Bringen Sie keine magnetischen Informationstr ger wie Kassetten oder Dis ketten in die N he des Magneten des Elektronenverschlusses des Spektrome ters Die Magneten sind sehr stark und k nnen die Informationstr ger besch digen Diffraktoren Caution Ber hren Sie nicht die gebogene Oberfl che der Diffraktoren Caution Ber hren Sie nicht oder versuchen Sie nicht die Oberfl che der Diffraktorenkri
48. ight 3 8 IbeX MAXrav User s Guide 136826C03 Index A AG Power 1 1 Accelerating Voltage 2 16 Acquire Menu 3 2 Peak to Background 2 39 3 7 Spectrum 2 15 2 28 Standards 2 31 3 7 Unknown Elements 2 34 Acquisition Information 2 16 3 2 Setup Saving 2 23 Active Window 2 2 Analog Rate Meter 3 3 Aperture 2 17 Automatic Peak Identification 2 11 Average Counts 2 27 Reading 2 26 B Background Color 2 9 Basic Operations 3 8 Beam Current 2 17 2 25 3 4 Voltage 2 17 Beginning Energv 2 20 2 22 Bias Scan 2 17 2 18 3 4 Voltage 2 18 3 4 C Cautions 1 1 Changing Display Colors 2 9 2 10 Changing the Display 3 6 Check Boxes 2 4 Clear Labels 3 6 Click and Drag 2 2 Closing the Program 3 2 Color 2 9 3 6 Comment 2 17 Configuration 3 3 Contract the Spectrum 2 7 Count Rate Counter 3 3 Cursor 3 4 D Data Entry Fields 2 5 Default Color Scheme 2 10 Define Elements in a Standard 2 30 Detectable Peaks 2 39 Detector 2 6 Bias 2 20 Bias Voltage 2 17 3 4 Diffractors 1 4 2 1 2 6 2 21 Options 3 3 Display Colors 3 6 Index 1 Index Displaving A Spectrum 2 7 Counts 3 3 Files 3 1 Rate Meter 2 27 Results 3 7 Two Spectrums 3 1 Drop Down Boxes 2 3 Dwell Time 2 20 2 23 E Edit Menu 3 2 Editing A Peak to Background File 2 41 A Standards File 2 34 An 2 35 Elapsed Time 3 3 Element Scan 3 2 Elements Unknown 3 7 EMSA Files 3 2 Ending Energy 2 22 Energy 2 20 Entering File Nam
49. ines Pr Me if EHE E Hs rt M Display line name Tine F Show satellite lines I Combine Kal Ka Threshold Select an element to label Click Table The periodic table of elements displavs Click once on an element Select the x rav lines to displav Click the check boxes of the x ray lines to include on the display The available x rav lines depends on the selected element e Click the All button to include all the available lines for the current element e Click the None button to remove all lines for the current element Select addition label display options for the current element e Display line name The x ray lines name e Show satellite lines The satellite lines e Combine Kal and Ka2 The Ka 1 and Ka2 lines are combined into one line labeled 2 14 IbeX MAXray User s Guide 136826C03 2 Using IbeX MAXrav Setting Up a Scan Acquisition KA These lines are typically very close together 5 Display x ray lines according to Relative Intensity Click the Threshold button 500 85 600 100 700 200 800 300 C 900 400 1000 Select an intensity value and then click OK Peak intensities are shown on the y axis of the spectrum The label for any intensity peaks below the threshold are not displayed 6 Apply the changes Click Close Setting Up a Scan Acquisition 136826C03 To collect data set up the microscope and sample set the acquisi
50. ions in the software The following is a description of each menu and the options in the menu File Menu 136826003 Save load and print from the File menu Open View or modify a previously saved file Open Overlay Display additional spectra files in the same display Up to two additional files can display by selecting Overlay 1 then Overlay 2 For more information see Changing Display Colors Overlay 1 Select the first spectral file to display Overlay 2 Select the second spectral file to display Save Periodically save the current file to a previously defined location Save As Save a file for the first time or save to a new directory location IbeX MAXrav User s Guide 3 1 3 Menu Reference Edit Menu Open EMSA EMSA is a standardized file format used to transfer data files from one x ray analyzer to another Use the Open EMSA option to load a spectrum that was saved using the EMSA format Save as EMSA Save a spectrum file in the EMSA format Print Print the current spectral file using the defined print option Print Options Define or modify the information to print on the report For more information see Acquisition Information Print Preview Display the defined report prior to printing Exit Close the IbeX MAXray program Edit Menu Edit and view the acquisition information and scan parameters Acquisition Information Specifv the Information to record during acquisition Scan
51. itative Analysis 1 From the Acquire menu click Peak Search Peak Search Centroid 1 739 keV Table i Si Kal Begin 1 728 keV End 11 753 keV Step eV LET Dwell 11 0 sec Start Record 1 728 1732 1 736 1 740 1 744 1 748 Close keV ti 2 Selectan element On the toolbar click the Table button 3 Begin the scan On the toolbar click the Start button The computed centroid displavs above the data 4 Record the peak search centroid Click Record to set the peak search energy value 136826C03 2 26 IbeX MAXray User s Guide 2 Using IbeX MAXrav Setting Up a Scan Acquisition 136826003 5 Exit Peak Search Click Close Rate Meter The rate meter displays the sum of all detected pulses at the current energy settings Use the rate meter to determine if an element of interest is present 1 From the Count menu click Rate Meter Counts per Second 710 304 7100 300 lt 2 3k 5 F 10k 30Kc 4 100k 300k Auto Ranging Max Rate 9 Reset FOn 17 s Smooth The count range on the left side of the dialog box 10k 100k 1k 10k 100k are graphed on the left y axis The count range on the right side of the dialog box 30k 300k 3k 30k 300k are graphed on the right y axis 2 Select a count range Select an energy level or one of the following option Auto Range A valid range is selected automatically Smooth Averages al
52. l counts Use this option if the counts are erratic e On The maximum rate intensity displays in the analog rate meter window and above the Reset button This option is ideal for determining if any counts are available Click Reset to clear the highest measure rate This value is also reset when you select a dif ferent range or the range changes IbeX MAXrav User s Guide 2 27 2 Using IbeX MAXrav Acquiring a Spectrum 3 Exit Rate Meter Click the Close button X in the upper right corner of the Rate Meter dialog box Counter The Counter displavs the sum of all counts over a defined time and for a defined energy 1 From the Count menu click Counter Counting Time sec 10 0 Counts lo Elapsed Time sec 0 0 sec Counts per Second 0 o e E Start the counter Click Start the counter displays the counts elapsed time and counts per second Click Stop to interrupt the counter The counter information displays During acquisition the number of counts measured elapsed time seconds and count rate counts per second display Exit Counter Click Close Acquiring a Spectrum After completing the Scan Setup you are ready for spectral acquisition ip From the toolbar click the Start button A confirmation dialog box displays Click Yes The graphs x axis represents the x rays energy in keV Large peaks indicate the presence of elements in the sample The graphs y axis repres
53. ndow Scale Overlav Scale the overlav spectrum to the foreground spectrum using the intensitv data surrounding the energv cursor Offset Overlav Displav or remove an offset view of the overlavs IbeX MAXrav User s Guide 3 5 3 Menu Reference Quant Menu Identify Peaks Perform a peak search and label the spectrum Peak Hints Display the Peak Hints dialog box Clear Labels Display or remove peak labels from memory Select Labels Define the element labels Modify Display Modify display information such as raw or smooth data black white or color line or histogram and thick or thin font Change Colors Change the display colors select a preset color scheme or modify the systems default color scheme Options include spectrum background overlay1 overlay 2 border surround peak labels numbers KLM markers and axis labels Sound Select the Sound option to turn on the computers audio hardware A check mark displays when this option is turned on To turn off the sounds select this menu option to remove the check mark Quant Menu Perform the sample analysis Create acquire and display standards Setup Standards Measure the elements weight concentration in the sample delete standards or change the standards composition values At least one standard must be defined for each element 3 6 IbeX MAXrav User s Guide 136826C03 3 Menu Reference Service Menu Acquire Standards Define the elemen
54. nt to scan or select one of the pre set user scan buttons For more information see Saving the Acquisition Setup 3 Select a Color option Select the color coding that the periodic table of elements Select by X ray Line to identify elements by energy lines Select by Diffractor to identify elements by the type of diffractor that is used to detect that element 136826C03 IbeX MAXrav User s Guide 2 19 2 Using IbeX MAXrav Setting Up a Scan Acquisition 4 Exit Periodic Table Click OK to save the changes and exit e Click Cancel to exit without saving the changes Scan Parameters Before acquiring a spectrum verify the microscope settings and make any necessary adjustments 1 From the Acquire menu click Setup Scan Setup Scan x Scan m Diffractor Beginning Energy 2 277 keV C MoB4C200 Ending Energy 2 337 keV C NiC80 Step Size ev WSib0 Dwell Time 1 00 sec C TAP Electronics PET i 2100 It Detector Bias volts F r SCA Baseline 2 01 volts C Automatic SCA Window 6 00 volts Parameters Cancel OK 2 Enter Scan and Electronics settings Click Elements and select an element from the periodic table of elements The following settings are entered for the selected element Make anv necessarv changes to these values Beginning Energy The scans minimum energy level in keV e Ending Energy The scans maximum energy level in keV e Step Size The spec
55. other microscope accessory except for those required by Thermo Electron Corpora tion Do not touch the spectrometer flow proportional counter window or the diffrac tors except as specified in the mounting procedures Do not touch the internal parts of the spectrometer with your hands or oils from the skin surface could contaminate the spectrometer and increase pump down time IbeX MAXrav User s Guide 1 3 1 Precautions and Safety Summary Safety Precautions Caution Do not scratch the O ring mating surfaces on the spectrometer or interface flanges Caution Do not place any magnetic media such as floppy disks near the magnets from the spectrometer electron trap The magnets are very strong and could damage the media Caution Do not change any of the IbeX MAXray adjustment screws without the help of an authorized Thermo Electron Service engineer Diffractors Caution Do not touch the face of the diffractors Caution Do not touch or attempt to clean the surface of any diffracting crystal The diffractor surfaces are sensitive and some can be dissolved with cleaning solvents including water Manual Gate Valve Option Never pump the column down with the gate valve closed and the spectrometer at atmosphere WARNING Do not open the gate valve when the SEM is at vacuum and the WD spectrometer is at air Opening the gate valve under these conditions could expose the microscope vacuum system to contamination If t
56. ron dazu aufgefordert werden Caution Die Sicherung im Elektrizit tsmodul mu der allgemeinen Stromspannung entsprechen IbeX MAXrav User s Guide 1 9 1 Precautions and Safetv Summarv Vorsichts und Sicherheitsanweisungen P 10 Gas Der Z hler der den proportionalen Flu mi t ben tigt ein spezielles Gas P 10 P 10 Gasflaschen k nnenbei Ihrem rtlichen Gash ndler erworben werden Die Gasflaschen sollten einen zweistufigen Regulator mit einem 1 4 NPT Anschlu haben damit der von Thermo Electron mitgelieferte Regulator zur dritten Stufe angeschlossen werden kann WARNING P 10 Gas ist GEF HRLICHES MATERIAL Benutzen Sie P 10 Gas nur in bereinstimmung mit den Sicherheitsanweisungen die Sie vom Hersteller erhalten WARNING Befestigen Sie die P 10 Gasflaschen an ein sicheres stabiles Objekt wie eine Wand oder Werkbank Die Gasflaschen beinhalten gef hrliches Material unter Druck Falls das Ventil besch digt wird oder der Mantel der Flasche undicht wird tritt eine gef hrliche Situation ein IbeX MAXrav Spektrometer Caution Der Arbeitsabstand des Spektrometers mu korrekt sein WD Spektrometer sind entworfen und hergestellt um mit einem speziellen Arbeitsabstand zur Probe zu arbeiten Lesen Sie in ihrer Gebrauchsanweisung zum Mikroskop nach welcher Abstand f r ihre Maschine empfohlen ist Caution Ein Hochspannungskabel verbindet die PCS Box mit dem WD Spektrometer Unterbrechen Sie diese Verbindung n
57. rungen zu entsprechen Das beeinhaltet eine Serie von Tests durch verschiedene Agenturen sowie alle Anforderungen um den h chsten Anspr chen zur Umweltvertr glichkeit gerecht zu werden Beachten Sie die folgenden Vorsichtsma nahmen um eine sichere Bedienung der Maschinen zu gew hrleisten Wechselstrom Elektrizit t WARNING Alle elektrischen Maschinen m ssen ber anwendbare Codes verf gen und d rfen nur von Thermo Electron Fachpersonal oder beauftragtem Fachpersonal installiert werden WARNING Im Inneren der Maschine befinden sich lebensgef hrliche Spannungen Hohe elektrische Spannungen befinden sich im inneren der Maschine Diese Spannungen k nnen schwerste Verbrennungen oder t dliche Elektroschocks ausl sen Fehler mit nicht korrekt geerdeten Maschinene k nnen hohe Spannungen an die Oberfl che transportieren e Verschiedene innere Komponenten arbeiten mit hohen Spannungen und d rfen weder isoliert noch abgedeckt werden Komponenten wie Kondensatoren oder Batterien k nnen hohe Spannungen beinhalten auch wenn die Stromzufuhr unterbrochen ist Sorgen Sie daf r da die Maschinen korrekt geerdet sind IbeX MAXray User s Guide 136826003 1 Precautions and Safetv Summarv Vorsichts und Sicherheitsanweisungen 136826C03 Schlie en Sie die Maschinen nur an korrekt geerdete Steckdosen an Wenn Sie unsicher sind lassen Sie die Steckdose von einem Fachmann untersuchen Schlie en sie ni
58. severe injurv or death CAUTION is used when the hazard or unsafe practice could result in minor injurv or propertv damage Other recommendations for product use are marked as IMPORTANT or NOTE Vour Thermo Electron equipment has been designed and tested to meet strict safetv requirements These include manv safetv agencies examinations and approvals as well as anv compliance to established environmental standards Heed the following precautions to ensure the continued safe operation of this equipment AC Power WARNING All electrical equipment must meet applicable codes and be installed bv Thermo Electron authorized support representatives WARNING Dangerous voltages are present inside the equipment High operating voltages are present inside the equipment These voltages can produce severe burns or fatal electrical shocks Failures in improperly grounded equipment can transfer dangerous voltages to outside surfaces Numerous internal components operate at high voltages and may not be insulated or shielded Components such as capacitors and batteries can store high voltages even with the power disconnected IbeX MAXrav User s Guide 1 1 1 Precautions and Safety Summary Safety Precautions WARNING Maintain proper equipment grounding Always connect equipment to a properly grounded power source receptacle If in doubt have the receptacle checked by a qualified technician Never use a ground adapter plug to
59. sition beam on Standard e Insert the Faraday Cup IbeX MAXrav User s Guide 2 33 2 Using IbeX MAXrav Quantitative Analvsis Enter the Beam Current Remove the Faraday Cup The acquisition begins The status of the acquisition displays at the bottom of the IbeX MAXrav window Acquisition stops automatically e Click Pause to temporarily stop the acquisition Click Continue to start the acquisition where it was stopped e Click Stop to end the acquisition prior the designated acquisition time 5 Save the standards file e Click Save Std Enter the standards file name and then click OK Standard files use the file extension std e Click Load Std to re acquire a previously saved standards file Click Print to print the currently displayed element information Acquire Unknowns Acquire Unknown counts in the sample for the elements defined in Acquire Standards To obtain accurate results it is assumed during the quantitative calculation that all elements in the sample have been included the total concentration is close to 100 If some elements have known weight percent concentrations enter these values as fixed concentrations for the quantitative result calculation and omit counting them It is possible to calculate the weight percent of one element of the sample by difference from 100 rather than performing a count for the element It is also possible to calculate the weight percentage of one of the five el
60. t m Color fol Color C Line Black amp White r Data qr Font C Raw C Thick Smooth Thin 2 4 IbeX MAXrav User s Guide 136826C03 2 Using IbeX MAXrav Starting IbeX MAXrav Text Fields Text fields have a white background Enter text bv clicking inside the field and then tvpe the text The example below shows one text fields The remaining boxes displav information that can not be changed but varies depending on the svstem settings or variables set in a different area of the software Counting Time sec 10 0 Text Field Counts 0 Displav Field Elapsed Time sec 0 0 sec Counts per Second 0 cme Cu Starting IbeX MAXray Start the lbeX MAXray software with the following procedure 1 Click the Microsoft Windows Start button select Programs and then click IbeX or MAXrav The main IbeX MAXrav window displavs imi NORAN Ibex ol x File Edit Acquire Count Settings View Options Quant Service Help Open Save Smooth Scale KLM 1genitv Labels Sean Start Stop 136826C03 IbeX MAXrav User s Guide 2 5 2 Using IbeX MAXrav Starting IbeX MAXrav Initializing the Svstem Each time the IbeX MAXray is turned off the diffractors and detector must be reset Initialization takes approximatelv 3 minutes For more information see Calibration Procedure 1 From the Service menu click Initialize Motors A message dialog box displavs 9 This could take a coupl
61. t menu click Acquisition Information IV File Name C Noran wDS data w_Siwds W Title ta Particle on VW Date Wednesday May 19 199 M Sample nl V Time 15 57 W Identification I Smoothed No 7 Commet RB Diffractor PET oo M Microscope feoLeso M BegnScan 1 700 k IV Beam Voltage fix 000 MeEndScan 182 kev I Beam Curent ind M StepSie 0002 ke IV Spot Size KI IV Dwell time 3 00 IV Aperture 2 j M Total Points 63 IV Magnification Raster ak IV Detector Bias volts IV SCA Baseline 1 00 volts M SCAwindow 600 yalts 2 Enter the acquisition information These settings must match the microscope The remaining parameters display for printing purposed only File Name The file name for the spectrum document Title A detailed description of the file e Sample A short description of the sample e Identification Sample identification 2 16 IbeX MAXrav User s Guide 136826003 2 Using IbeX MAXrav Setting Up a Scan Acquisition 136826003 Comment Miscellaneous remarks about the sample or acquisition Microscope The microscope model Beam Voltage The voltage that produces the electron beam in keV Beam Current The microscopes beam current in nanoamps nA Spot Size The electron beams spot size Aperture The aperture of the microscope objective Magnification The magnification value 3 Select the inform
62. the IbeX MAXrav optic is inserted without knowing its position Driving the stage into the optic will damage the optic Caution The controller must be installed according to the procedures described in the installation and service manual to avoid damage to the spectrometer Caution The fuse s in the controller must match the line voltage Caution Check that the fuse s for the input AC voltage are correct IbeX MAXrav User s Guide 1 5 1 Precautions and Safety Summary Safety Precautions The switching power supply has a universal input autoranger that eliminates the requirement of changing jumper wires or switches to change the input voltage range but the correct fuse s must be installed e For 100 120 VAC operation use one T 250V 3A fuse For 230 240 VAC operation use two T 250V 2A fuses 5x20 mm Caution For continued protection against fire replace the fuse s only with the specified type Caution Do not place objects under or around the bottom of the controller that would restrict the cabinet cooling Never operate vour Thermo Electron equipment if vou notice unusual noises or foul odors Disconnect the power cord from the main power source and call vour local Thermo Electron support specialist Caution Make sure the P 10 gas flow through the proportional counter is correct before energizing the detector Flow Proportional Counter Window The material that isolates the gas inside the detector from the v
63. tion parameters and then acquire the spectrum To re acquire or review a previously saved spectrum load the saved file and then edit as needed Microscope and Sample Before preparing the microscope and sample read the safety precautions in Chapter 1 1 Selecting a sample Use a sample free of oils and particles to reduce the chance of contaminating or corroding the microscope chamber or detector Well polished smooth surface produces the best results X ray absorption varies when using a rough surface and reduces the accuracy of your results 2 Insert the sample and evacuate the chamber Do not bump the spectrometer with the sample or expose the spectrometer to a sudden changes in pressure IbeX MAXrav User s Guide 2 15 2 Using IbeX MAXrav Setting Up a Scan Acquisition Acquisitions are sensitive to sample position and angle 3 Setthe microscopes accelerating voltage Set the accelerating voltage to at least 1 1 2 times the highest spectral peak 4 Obtain an image of the sample A small scan area improve the most accurate results Zoom in to a higher magnification or select the Spot Mode on the microscope Not all microscope are equipped with the spot mode feature For more information see vour microscopes user manual Acquisition Information Acquisition information remains the same from scan to scan until it is modified and is saved with a file The report content is selected in this window 1 From the Edi
64. trometer step size during acquisition in eV Dwell Time The dwell time on each step of the scan in seconds e Detector Bias The optimum detector voltage for the bias scan For more information 2 20 IbeX MAXrav User s Guide 136826003 2 Using IbeX MAXrav Setting Up a Scan Acquisition see SCA Scan e SCA Baseline The optimum detector baseline voltage for the SCA scan Optimize this value to reduce noise The sum of SCA Baseline and SCA Window must not exceed 8 4V See diagram below SCA Window The optimum range of detection for the SCA scan in volts By optimiz ing this value you can reject counts produced by noise The sum of SCA Baseline and SCA Window must not exceed 8 4V See diagram below LLD jor volts End je4 volts Step 2 volts Dwell fo sec Window faz volts Bias 2300 7 volts Close SCA Window 3 Select a Diffractor A diffractor within the Beginning Energy and Ending Energy field must be selected The available diffractors vary from system to system From the Settings menu click Configuration A window listing the diffractors and cor responding energy ranges Select a diffractor by its energy ranges Configuration NORAN IbeX Demonstration Model Ix Diffractor 2d spacing A Energy Range keV MoB4C200 200 000 0 066 to 0 256 NICEO 0 000 0 165 to 0 641 e Select Automatic to have IbeX MAXrav select the best diffractor 136826003 IbeX MA
65. ts weight concentrations in the sample or count the standards for these elements Enter the elements composition Edit Standards prior to selecting this option Acquire Unknowns Count the defined elements in the sample Acquire Peak to Background The peak to background option identifies the absents or presents of an element This indication reflects the relative concentration of that element compared to the background Results Select the matrix correction method This method is used to calculate each elements weight percentage Service Menu Most options on the Service menu are used by Thermo Electron service engineer and are password protected Initialize Motors Reset the detector and diffractors starting position This operation must be preformed whenever the system is restarted Password Password provides access to the remaining Service menu options Contact your service representative for more information Help Menu 136826003 Access information about the IbeX MAXray program from the Help menu Introduction General information on the IbeX MAXray program Navigating Information on how to navigate in the IbeX MAXray program IbeX MAXrav User s Guide 3 7 3 Menu Reference Help Menu How To Information on how to preform basic operations in the IbeX MAXrav program Menu Commands Information on commands associates with each menu item About Information on the IbeX MAXray program version and copyr
66. zten Anschlu bevor Sie das SEM l ften Wenn Luft oder Stickstoff in die Kammer dringen kann das Fenster des proportionalen Z hlers leicht zerbrechen 1 14 IbeX MAXrav User s Guide 186826003 2 Using IbeX MAXrav The IbeX MAXray is designed to analvze one elemental x ray line for each diffractor Nearby lines are measured depending on the energy Up to six diffractors are mounted on the turret For more information on how the diffractors work see Theory of Operation in this manuals appendix A 1 Software Controls and Layout The following sections describe software operations such as mouse functions access features and terminology Menu Bar The menu bar is at the top of the main window The menus contain options for setting up displaying and operating the IbeX MAXray software Clicking once on a menu name displays the options File Edit ROMEA Count Settings View Options Quant Service Help Element Scan Scan an Setup Peak Search Start Scan Stop Scan Pause Scan Toolbar The toolbar is a row of shortcut buttons located below the menus Each shortcut button corresponds to a menu option 136826003 IbeX MAXrav User s Guide 2 1 2 Using IbeX MAXrav Software Controls and Lavout Microsoft Windows NT Tools Most Windows applications displav similar features and applications The following diagram labels the window Maximize the Window restore from icon Minimize the Window re

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