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Bruker QUANTAX EDS Скачать руководство пользователя страница 51

5.1 Preparatory Steps

QUANTAX EDS

51

This chapter gives the analyst an overview of the most important tools of the ESPRIT
software, permitting a quick start to perform analyses with the QUANTAX EDS system.

The procedures described here assume standard (default)  ESPRIT settings. They also
refer to  the  use  of  a scanning electron microscope (SEM)  or  a scanning transmission
electron microscope (STEM) or similar.  Differences in the analysis of bulk samples
(mainly SEM and FIB) and electron transparent samples (TEM, STEM, sometimes SEM or
FIB) are pointed out.

5.1

Preparatory Steps

This section describes the actions needed prior to starting the analytical work with the QUANTAX

EDS system.

Step

Examples/hints

1

Prepare the sample and place it in the

microscope

e.g., embedding, polishing and carbon

coating, TEM sample preparation

2

Adjust high voltage and working distance

(SEM) or eucentric height (TEM) on the

microscope. Switch on the beam. Adjust
magnification.

Choose high voltage (HV) based on
overvoltage of elements to analyze.

3

Start ESPRIT and log in.

Refer to section 4.1.

4

Use the

icon in the bottom left

corner of the

Microscope

configurator to

open the

MICROSCOPE

CONFIGURATION

dialog and check the

settings.

WD, Magnification, HV values must match
values set on the microscope (see section

4.5.3). Device status indicator should be
green.

5

Use the

icon in the bottom left

corner of the

EDS

configurator to open

the

EDS CONFIGURATION

dialog and

a) Set

Pulse throughput

and

Maximum

energy

Normal operation mode

should be selected.

For

Pulse throughput

and

Maximum

energy

use

Automatic

settings. Change it on

demand.

b) Check

Detector temperature.

Check operation temperature. Device status

indicator should be green (see section 4.5.5).

6

Check input count rate and dead time for

the analysis.

The input count rate should be chosen

according to the analytical task.

7

Use the

icon in the bottom left

corner of the

Sample

configurator to

open the

SAMPLE PROPERTIES

dialog

and set sample name and description.

The sample name applies for all further
measurements.

8

Proceed with required analysis.

Refer to section 5.7, 5.14, 5.15 or 5.17.

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Содержание QUANTAX EDS

Страница 1: ...QUANTAX EDS Energy dispersive X ray spectrometer for electron microscopy User Manual ...

Страница 2: ...e checked the contents of this manual for agreement with the hardware and software described Since deviations cannot be precluded entirely we cannot guarantee full agreement However the data in this manual are reviewed regularly and any necessary corrections are included in subsequent editions Suggestions for improvement are welcome Order no DOC M82 EXS066 2015 Bruker Nano GmbH Berlin Germany All ...

Страница 3: ...nic Units 20 3 3 3 Software and Data Handling 21 4 The ESPRIT 2 Software 23 4 1 Start up and Login 25 4 2 User Administration 26 4 3 Workspaces 28 4 4 Display Control 29 4 5 Configurator Bar 31 4 5 1 Sample Configuration 32 4 5 2 Standards Configuration 32 4 5 3 Microscope Configuration 33 4 5 4 Scan Configuration 34 4 5 5 EDS Configuration 36 4 5 6 Additional Configurators 37 4 5 7 Report 38 4 5 ...

Страница 4: ... 78 5 12 Quantitative EDS Analysis of Bulk Samples 81 5 12 1 Using the Method Editor 81 5 12 2 Standardless Quantification 83 5 12 3 Standard based Quantification with a Temporary Reference 86 5 12 4 Standard based Quantification with Standards Library 88 5 13 Quantitative EDS of Electron Transparent Samples 90 5 13 1 Standardless Cliff Lorimer Quantification 90 5 13 2 Standard based Cliff Lorimer...

Страница 5: ...t both the needs of the novice as well as the experienced user All QUANTAX systems ESPRIT software includes an online help system and supports remote diagnosis and assistance via the Internet This manual provides a general software overview and a practical step by step description of the most common measurement procedures that can be performed with the QUANTAX EDS system The integrated assistants ...

Страница 6: ......

Страница 7: ...2 Safety Information 2 1 Radiation Safety 9 2 2 Beryllium 10 2 3 Electrical Safety 10 2 4 Electromagnetic Compatibility 11 ...

Страница 8: ...User Manual 2 Safety Information 8 ...

Страница 9: ...and material damage arising from non intended usage 2 1 Radiation Safety Changes to the original detector installation are strictly prohibited Radiation safety may be impaired by improper installation or de installation The QUANTAX microanalysis system uses the X radiation that is generated by sample interaction with electrons from the electron source of the microscope or photons emitted by the op...

Страница 10: ...d collect them using pieces of adhesive tape The waste has to be labeled and disposed of according to the local safety hazard regulations Wear a filter mask during cleaning up 2 3 Electrical Safety High voltage inside Do not remove covers All parts have been designed according to the safety requirements for electrical equipment for measurement control and laboratory use or the European Low Voltage...

Страница 11: ... regarding electromagnetic immunity of general electronic equipment This is not a disadvantage under normal circumstances because the QUANTAX system works under the same conditions as electron microscopes and the laboratory environment is designed to meet the requirements of these instruments Bruker devices fulfill all requirements regarding active electromagnetic compatibility emission rules ...

Страница 12: ......

Страница 13: ...3 The QUANTAX EDS System 3 1 Hardware System Components 15 3 2 ESPRIT 2 Software 18 3 3 General Operating Instructions 19 ...

Страница 14: ...User Manual 3 The QUANTAX EDS System 14 ...

Страница 15: ...individual pulse heights are a statistical measure of the corresponding quantum energy By digitally recording and counting a great number of such pulses within a so called multi channel analyzer MCA a complete image of the X ray spectrum is built up almost simultaneously This digital quantum counting technique makes the energy dispersive spectrometry extremely reliable Bruker XFlash Detector The B...

Страница 16: ...used refer to the detector s hardware manual for specifications Faster than optimum shapers can be selected at the expense of energy resolution which is acceptable for ultrahigh speed applications like element mapping The QUANTAX spectrometer electronics is configured according to the chosen detector and QUANTAX system level 3 1 3 Spectrometry Data Interface and EM Control Data interface The propr...

Страница 17: ...s RS232 are also provided 3 1 4 Computer Workstations Client server architecture All QUANTAX systems feature client server architecture The server part controls the spectrometer and microscope hardware and performs basic data evaluation the client system is what is visible to the user and provides the graphical user interface GUI Client and server can share one computer or run on different compute...

Страница 18: ... ESPRIT the user is prompted to provide this CD for registration The license file Licence pdf is stored to the server computer after completion the license CD should be kept in a safe location Software options Licenses control general access to the ESPRIT software as well as installed options Selected options or the complete license can be time limited Updated license files obtained from Bruker Na...

Страница 19: ...g to the type of detector at hand different operations regulations apply These must be followed strictly After complete shutdown of the XFlash detector an extended warmup period and or energy channel recalibration see section 5 2 may be necessary for high precision measurements XFlash detectors Bruker XFlash detectors are maintenance free There is no additional wearout caused by permanently poweri...

Страница 20: ...ndow is contaminated contact customer support or your local supplier for assistance 3 3 2 Electronic Units Setup Unauthorized changes to the electronic and electric installation are not permitted Besides safety regulations see section 3 1 2 also electromagnetic immunity and noise pick up issues are addressed during installation Note that electronic parts may have to be adapted to the local mains v...

Страница 21: ...QUANTAX system is installed on special selected and configured computers Any change of the system configuration user status access rights or else can impair system integrity Also new applications especially multi media internet and game software can interfere with QUANTAX The internal client server architecture of QUANTAX depends on Windows communication services that may be adversely modified by ...

Страница 22: ......

Страница 23: ...Software 4 1 Start up and Login 25 4 2 User Administration 26 4 3 Workspaces 28 4 4 Display Control 29 4 5 Configurator Bar 31 4 6 Loading and Saving Data and Results 39 4 7 System Functions 41 4 8 The Help System 47 ...

Страница 24: ......

Страница 25: ...f the corresponding option is checked The name of the last user is always retained Multi user systems On multi user systems several users can access manage and evaluate private and shared data simultaneously The unique user name and password will give access to the private data and settings Select the server to log in from the pull down menu below after clicking on the arrow symbol of the button A...

Страница 26: ...g the Bruker icon in the Windows system tray opens the console of the communication server The tab QUANTAX user lists the current assigned users A new user can be added after clicking the button A password can be entered leaving the field empty is permitted and an optional user description can be added As user type User Main user and Supervisor can be selected User has limited access to the ESPRIT...

Страница 27: ...AX communication server After clicking the deletion of the user data has to be confirmed separately Caution once confirmed the deletion cannot be revoked If deletion of the data is not confirmed the data are retained invisibly a new user with the same name as a previously deleted will be assigned to the idle data The number of assigned measure client ports determines how many users can log in simu...

Страница 28: ... 4 3 1 ESPRIT workspace list in normal fullscreen and large style buttons mode The name of each workspace is displayed on the icon if the Large style buttons checkbox under System Appearance is activated Assistants gives access to a step by step guide for common analysis procedures Spectra allows spectrum acquisition and analysis of saved X ray spectra Objects permits point multipoint and area EDS...

Страница 29: ...ol and running unattended fully automatic analysis tasks Scripting permits writing and running user defined scripts System is used to adjust global settings and calibrate the X ray spectrometer and image system Additional functions display settings language font size license management communication with electron microscope and motorized sample stage 4 4 Display Control Program window and title ba...

Страница 30: ...ll parts of the configurator bar are described in detail in section 4 5 Image capture chart The workspaces Objects Line scan Mapping and Imaging have a dedicated chart for controlling the electron image capture Analysis spots objects scan lines and mapping areas can be defined on the captured image Image capture is controlled directly from the current workspace Additionally a special window for fa...

Страница 31: ...ailable in the QUANTAX system The number of configurators that actually appear on the screen depends on the license and may differ from the images shown in this manual The individual configurators display relevant adjustable parameters of the sample standard libraries X ray excitation sources scan unit spectrometers and other detectors as well as the report and project tools They will be explained...

Страница 32: ...s up Before measurement general properties of the sample can be entered in this dialog All subsequently collected data spectrum image line scan map will contain these parameters Default input parameters are name and description Additional user defined data can be added clicking the icon Sample coating If the sample is coated to enhance electrical conductivity this can be entered under Sample coati...

Страница 33: ...oscope configurator select entry menu The Microscope configurator displays the main parameters of the electron microscope Magnification Image magnification set on the electron microscope High voltage Acceleration voltage set on the electron microscope WD working distance Sample pole piece distance mm Stage X Y Z Microscope stage position coordinates are displayed if available The parameter to be d...

Страница 34: ...on capability This is recommended when performing EBSD analysis using large tilt angles to correct image distortion of microscope images element or orientation maps 4 5 4 Scan Configuration Fig 4 5 10 Scan configurator Fig 4 5 11 Scan configurator select entry menu The Scan configurator displays the scanning parameters Image resolution Image size in pixels Dwell time Signal collection time of a si...

Страница 35: ...ides noise reduction and expanded image scan time while limiting the increased stress on the sample by maintaining a high scan speed The line average factor will multiply the total image acquisition time The total Image capture time is calculated and displayed Mapping The Dwell time is the time the electron beam stays on a pixel while acquiring an EDS map The Line average factor for mapping contro...

Страница 36: ...orner of the EDS configurator indicates the status of the instrument A green rectangle means that the detector is activated and ready to use a red rectangle indicates that the detector is idle Toggling between activated and deactivated states can be achieved by clicking on the EDS configurator When clicking on the icon in the bottom left corner of the EDS configurator the EDS DETECTOR CONFIGURATIO...

Страница 37: ...rs Motorized detector axis If the EDS detector is equipped with a motorized axis the icon in the bottom left corner of the EDS configurator see Fig 4 5 17 displays and controls the position of the EDS detector The icon shows one of the two states The EDS detector is inserted and is at measurement position if the icon is displayed The system is ready for use When clicking on the icon in this status...

Страница 38: ...rts the number of pages objects and the name of the selected report Clicking on the icon in the bottom left corner of the Report configurator opens the report editor Further details on how to use the report function are described in section 5 21 4 5 8 Project Fig 4 5 19 Project overview The Project tool serves as data clipboard for data transfer between ESPRIT workspaces or save all data added to ...

Страница 39: ...ename or select a file in the list A preview image and an info box will be displayed if applicable The private data volume on the QUANTAX server is selected via the topmost icon labeled with the user name To open the shared server folder or access the local or network drives click the button labeled Public or a drive letter in the list below In client server installations local and network drives ...

Страница 40: ...the Windows clipboard To export graphical data to files use the option Save under the subsection Graphic Image Map image To exchange graphics via the Windows clipboard click Copy in the according subsection of the Import Export menu or in the local menu after a right mouse click into the corresponding window area Projects Storing data in a project and saving the whole project to a project file is ...

Страница 41: ...ter Imaging WDS Microscope and Stage Fig 4 7 1 Workspace System 4 7 1 System The section System provides product information user license administration and control of the spectrometer settings All items in this section are generally only of interests to Bruker service personnel Unless explicitly requested please do not alter any parameters within the system assignments System report This area lis...

Страница 42: ...etup of the X ray spectrometer s and other devices are normally only performed during system installation The assignment is completely automatic Each detector to be assigned must be connected to either Bruker MegaLink port a RS232 port an USB port or via Ethernet of the QUANTAX server and powered on when the button is clicked All available ports are automatically scanned for valid connections Once...

Страница 43: ... 0 and Inverted TIFF assigns white to 0 In the subsection Miscellaneous options the user can activate deactivate the Large style buttons mode If the checkbox is activated the name of the workspace or function is shown on the icon e g The Auto close delay option defines the time the mouse over hint messages of the icons are displayed The Colors for overlay objects in different workspaces can be sel...

Страница 44: ...of the energy axis abscissa on the EDS spectrum using a calibration sample more later with known composition The calibration is recommended for high precision quantitative analysis or in instances where the line markers do not match the peak positions or if the auto identification fails Pulse throughput and Range selection The user can choose the different combinations of pulse throughput and ener...

Страница 45: ...e to show the sizing handles then drag the handles to fine tune the position of the end points of the line Fig 4 7 6 Stage calibration setup Once confirmed enter the correct certified values of the line length in µm Click the button to store the according calibration value Stage calibration This option calibrates the stage movement alongside the SEM image for montage purposes Before stage calibrat...

Страница 46: ... the overlap in the X direction the same applies to Y The rotation will change the relative rotation between adjacent fields In the image the red curly brackets highlight the misaligned overlaps Adjust the overlaps and rotation in small steps Care should be taken to focus not on the corners of the image overlaps but at the straight edges in the corners the image distortion is at its worst Fig 4 7 ...

Страница 47: ...nnels e g SE BSE HAADF It is not advised for users to modify the other settings in this section unless explicitly advised by Bruker Service personnel 4 7 7 Stage The limits must not be changed without informing Bruker Service personnel To verify the stage limits select the tab The stage limits for the SEM are set during installation of the QUANTAX system 4 8 The Help System Help system ESPRIT feat...

Страница 48: ......

Страница 49: ...ting Correction 68 5 10 System Factor Calibration Beam Current Setting 70 5 11 Standards Library 73 5 12 Quantitative EDS Analysis of Bulk Samples 81 5 13 Quantitative EDS of Electron Transparent Samples 90 5 14 Object Analysis 96 5 15 Line Scan 98 5 16 Quantitative Line Scan QLine 100 5 17 Map Acquisition 102 5 18 Quantitative Mapping QMap 104 5 19 Map Processing 106 5 20 Phase Analysis 109 5 21 ...

Страница 50: ...User Manual 5 Step by Step Guides 50 ...

Страница 51: ...high voltage HV based on overvoltage of elements to analyze 3 Start ESPRIT and log in Refer to section 4 1 4 Use the icon in the bottom left corner of the Microscope configurator to open the MICROSCOPE CONFIGURATION dialog and check the settings WD Magnification HV values must match values set on the microscope see section 4 5 3 Device status indicator should be green 5 Use the icon in the bottom ...

Страница 52: ...User Manual 5 Step by Step Guides 52 Fig 5 1 1 Preparatory steps for measurements with the ESPRIT software ...

Страница 53: ...ion Preferably use single element standards e g pure copper to avoid peak misidentification improve speed and accuracy 3 Set the beam current to produce an intermediate count rate Use microscope controls Set appropriate magnification on a homogeneous sample area 4 Select element and spectral line for calibration Use Kα lines whenever possible 5 Click to check the current energy channel calibration...

Страница 54: ...User Manual 5 Step by Step Guides 54 Fig 5 2 1 Spectrometer calibration ...

Страница 55: ...s if needed 7 Click on the button to set capture parameters and Image number or Automatic numbering The image will have the name set in the Sample configurator Choose Single to acquire one image frame Continuous to update image frames or Sliding average to average a number of frames 8 an image 9 Image legend parameters can be edited using the icon The image name can also be changed here after capt...

Страница 56: ...User Manual 5 Step by Step Guides 56 Fig 5 3 1 Image capture ...

Страница 57: ...d oscilloscope overlay tools if needed 4 Click on the button to open the Capture parameters menu 5 Set Image number or Automatic numbering 6 Select Activate in the Image extension submenu 7 Set Width and Height E g 2 x 3 means that 2 images in x direction and 3 images in y direction will be captured The current stage position is in the center of the mosaic image 8 the extended image 9 Use the imag...

Страница 58: ...User Manual 5 Step by Step Guides 58 Fig 5 4 1 Image extension ...

Страница 59: ...ing the analysis or use a lower Special value than used for Imaging to save time 4b When acquiring a Map the correction time is equal to the Mapping scan time If image drift is extensive reduce Image capture time by decreasing Mapping Dwell time and Line average 5 Click on to change parking position of the beam Use a parking position outside of the analysis area to avoid beam induced contamination...

Страница 60: ...User Manual 5 Step by Step Guides 60 Fig 5 5 1 Image drift correction ...

Страница 61: ...urements on images using the tool and display results as table 5 Apply filters or perform other operations Drag intermediate images to the clipboard shown as thumbnails at the bottom of the workspace 6 Use the workspace icon to a Save processed image Use rti file format to save all available EM images processed image result tables and drawn items into one file b Add processed image to project Alte...

Страница 62: ...User Manual 5 Step by Step Guides 62 Fig 5 6 1 Image processing ...

Страница 63: ...nts Exhaustive 1 000 000 counts for elements close to the detection limit Manual If Manual is selected the acquisition has to be stopped manually by clicking the button Real Time The acquisition will stop after the time entered in the dialog box has elapsed Live Time The acquisition will stop after the dead time corrected acquisition time has elapsed Counts The acquisition will stop after the pred...

Страница 64: ... to be saved manually see section 5 22 b Add data to report 7 Use the spectrum chart icon to a Save spectrum or result list element selection graphic Highlight spectra in the spectrum list to save several spectra Alternatively right click into the spectrum Various file formats are possible To include all meta data use the spx format Refer to section 5 8 and 5 12 1 b Add item to project Alternative...

Страница 65: ...ked in the menu 1f Results Click to select Spectrum information identification or Display of quantification results Mass Mass norm Atom Stoich Stoich norm 2 Multiple spectra can be selected checkbox or highlighted by clicking on the spectrum line gray outline Checkbox selects spectra for display highlighted spectra can be processed and exported To highlight several spectra use SHIFT or CTRL keys a...

Страница 66: ...difference relative difference quotient maximum and minimum The resulting spectrum will be added to the spectra list 11 Click the icon to select or de select an element Any element can be selected or de selected just by clicking the according symbol 12 Select the tab in the periodic table The Finder option supports the identification of unknown peaks in the spectrum Place the spectrum cursor over ...

Страница 67: ...5 8 Using the Spectrum Chart QUANTAX EDS 67 Fig 5 8 1 Features in the spectrum chart ...

Страница 68: ...ntification in subsequently acquired spectra line scans and maps Acquire a coating correction file of a coated sample and use this to subtract from all subsequent spectrum acquisitions 4 a spectrum of a coated sample as coating reference Make sure that the sample does not contain the same element as the coating material 5 Perform quantification of the spectrum Refer to section 5 12 2 6 Click on an...

Страница 69: ...5 9 Sample Coating Correction QUANTAX EDS 69 Fig 5 9 1 Sample coating correction Step 1 to 8 Fig 5 9 2 Sample coating correction Step 9 to 11 ...

Страница 70: ...s Use a single element calibration sample Co Mn Cu Select a homogeneous area for spectrum acquisition 2 Load or create a standards library Follow section 5 11 1 3 Click the Standards configurator s calibration icon to open the SYSTEM FACTOR CALIBRATION dialog 4 Select the material of the Calibration sample from the Select the sample to use for calibration drop down list 5 Set Acquisition time para...

Страница 71: ...Load or create a standards library Follow section 5 11 1 for bulk samples or sections 5 11 2 and 5 11 3 for electron transparent samples 3 Click the Standards configurator s calibration icon to open the SYSTEM FACTOR CALIBRATION dialog 4 Enter probe beam current value manually in the System factor field and press Enter For Zeta quantification of electron transparent samples the probe current needs...

Страница 72: ...User Manual 5 Step by Step Guides 72 Fig 5 10 2 Beam current setting ...

Страница 73: ...a spectrum spx which was acquired with the corresponding detector geometry ii Select No If you are using the ESPRIT software connected to the microscope Update standards library with standard spectra 3 Perform system factor calibration Follow section 5 10 4 Move the reference sample into analysis position and a reference spectrum within the Spectra workspace Follow section 5 7 to acquire a spectru...

Страница 74: ...F STANDARD LIBRARY dialog 10 Click on an element to select it 11 Select the standard spectrum assigned to the selected element The assigned spectrum appears in spectrum chart 12 Click to change standard concentrations The EDIT STANDARD dialog pops up where the assigned concentrations can be changed 13 Click to re quantify the standard spectrum The QUANTIFICATION dialog pops up where the re quantif...

Страница 75: ...5 11 Standards Library QUANTAX EDS 75 Fig 5 11 2 Quantification dialog ...

Страница 76: ...try parameters do not match proceed with step 3 If they match proceed with quantification as described in section 5 13 1 or 5 13 2 3 Use the standards library icon to a Load a standards library or Load a previously saved esl file which corresponds to detector geometry parameters Proceed with step 5 b Select New to create an empty standards library The question Do you want to load a spectrum measur...

Страница 77: ...ed to calculate theoretical factors or set standards as described in section 5 13 2 7 Use the standards library icon to save the standards library Save the standards library containing Cliff Lorimer factors as esl file steps can be omitted Fig 5 11 3 Maintain standards library for Cliff Lorimer factors ...

Страница 78: ...m parameter double click on the highlighted line of the active spectrum in the spectrum list below the spectrum to open the SPECTRUM PROPERTIES dialog and enter the beam current in pA as system factor in the Parameter tab a a spectrum b Use the Spectrum chart icon to open a spectrum 3 Follow the standardless quantification steps 6 to 13 to identify elements set background regions and deconvolution...

Страница 79: ...t Zeta Factors to Standard Follow this guide to update Zeta factors for all elements by performing a polynomial fit based on Zeta factors of elements set using standard sample s Step Example hints 1 Set up Zeta factors for the standard sample Follow section 5 11 3 Experimental Zeta factors and see Fig 5 11 4 2 Click the icon in the bottom left corner of the Standards configurator to open the ADMIN...

Страница 80: ... based on the already existing standard composition values A polynomial is fitted on the standard elements Zeta factors Zeta factors for elements not contained in the standard sample s are interpolated 6 Press to confirm the new Zeta factors 7 Use the updated Zeta factors for quantification Follow section 5 13 3 Fig 5 11 5 Fitting the Zeta factors to standard ...

Страница 81: ...the Elements menu to a choose how peaks will be labelled Use spectrum elements will use element markers that you have previously set in the spectrum via the icon Use list elements will only use the elements that you have selected bold in the periodic table within the method editor Search additional elements will perform an AutoID see also step 4c b access element properties Double click or right c...

Страница 82: ...s menu Use Series fit as default 8 Select the Quantification model menu Use PB ZAF as default Use Rho Z for light elements See section 5 13 1 5 13 2 and 5 13 3 for further reference 9 Use the Additional settings menu for a Setting high voltage correction Click to perform automatic high voltage or sample tilt angle correction b Setting sample tilt angle correction c Selecting fast quantification 10...

Страница 83: ...This step can be omitted 5 Start quantification by clicking the button If quantification is set to automatic the quantification results appear in the spectrum list see section 5 7 If quantification is set to interactive the QUANTIFICATION dialog pops up In this case proceed with step 6 6 Edit quantification parameters using the quantification dialog The left dialog part has the same functionality ...

Страница 84: ...art Compare deconvolution results with measured spectrum 15 Review quantification result table 16 Click a to load a quantification method Use this to load a previously saved or a default quantification mtdx file b to save current settings as a quantification method Use this to save the current settings as quantification method mtdx file Alternatively use on the button c to add a method with curren...

Страница 85: ...5 12 Quantitative EDS Analysis of Bulk Samples QUANTAX EDS 85 Fig 5 12 2 Automatic standardless quantification ...

Страница 86: ...ng or rename spectrum after acquisition 5 Click at the button and select Load Load a quantification method 6 Set Method mode to Interactive 7 Click The QUANTIFICATION dialog opens Set quantification parameters Element ID EDS background Deconvolution as needed 8 Click EDIT STANDARD PROPERTIES dialog opens 9 Enter reference concentrations and click NOTE The reference values are TEMPORARILY stored un...

Страница 87: ...od editor and select Use standards under Quantification model 16 Click unless automatic quantification during or after acquisition is enabled 17 Use the button of the result table to Copy Save or Add to project or Add to report Save the modified quantification method for further use Use on the button or Save in the quantification dialog Fig 5 12 3 Standard based quantification with temporary refer...

Страница 88: ... factor calibration Refer to section 5 10 3 Select the or workspace and This workflow also applies to any spectrum chart available in the ESPRIT software a a spectrum Follow section 5 7 b Use the Spectrum chart icon to open a spectrum Optionally drag and drop a spectrum from the Project into the spectrum workspace 4 Click on the button and select Load to load a quantification method Select a stand...

Страница 89: ...5 12 Quantitative EDS Analysis of Bulk Samples QUANTAX EDS 89 Fig 5 12 4 Standard based quantification with a standards library ...

Страница 90: ...the project to the spectrum chart Two different quantification methods can be loaded the active one is displayed in bold 4 Make sure that geometrical EDS detector and HV parameters of spectrum and Cliff Lorimer factor database standards library match If the information message Cliff Lorimer Zeta factor Wrong primary energy in standards library pops up update the standards library as described in 5...

Страница 91: ...X EDS 91 9 Use the icon of the result table to Copy Save or Add to Project or Add to report Save the modified quantification method for further use Use on the button or the button in the quantification dialog Fig 5 13 1 Standardless Cliff Lorimer quantification ...

Страница 92: ... 13 1 Set quantification Method mode to Interactive to access the QUANTIFICATION dialog 4 Click The EDIT STANDARD PROPERTIES dialog pops up 5 Enter reference element concentration values for standard sample Use Mass or Atomic 6 Click The VALIDATION dialog pops up with new and old Cliff Lorimer factors 7 Select an element as reference The CL factor of this element will not be changed Advice Keep a ...

Страница 93: ...5 13 Quantitative EDS of Electron Transparent Samples QUANTAX EDS 93 Fig 5 13 2 Standard based Cliff Lorimer quantification ...

Страница 94: ...ighted line of the active spectrum in the spectrum list below the spectrum to open the SPECTRUM PROPERTIES dialog and enter the beam current in pA as system factor in the Parameter tab c drag and drop a spectrum from project to Spectrum chart 5 Click on the button and Load a quantification method Select a TEM quantification method Alternatively drag and drop a quantification method from the projec...

Страница 95: ...5 13 Quantitative EDS of Electron Transparent Samples QUANTAX EDS 95 Fig 5 13 3 Standard based Zeta quantification ...

Страница 96: ...ation is desired check if automatic analysis After acquisition or Continuous is selected 7 a spectrum Objects are automatically acquired in sequence Progress is indicated by the acquisition bar If Manual is selected the acquisition has to be stopped manually 8 The acquired spectra will appear in the spectrum list Refer to section 5 8 for further reference 9 Use the workspace icon to a Save object ...

Страница 97: ...5 14 Object Analysis QUANTAX EDS 97 Fig 5 14 1 Object analysis ...

Страница 98: ...se the Finder in the Spectrum tab Identified elements are displayed in the line profile thumbnail bar The element selection can be changed at any time during or after the line scan acquisition 8 Select elements in the thumbnail bar by ticking the boxes below the individual element images to display their profiles in the Profiles tab Optionally use or on the right of the thumbnail bar Use the icon ...

Страница 99: ...an menu Confirm the pop up window Do you want to save point spectra too by clicking to transfer spectral data c Add data to report 12 Use the thumbnail bar icon to Add Line scan to report Highlight elements in profile thumbnails Select Individual element profiles to add separate profiles for each element Select Composite element profile to add all selected elements in one diagram and the scan imag...

Страница 100: ...o change profile display options Select from Counts Net sum Mass percent Mass percent norm and Atomic percent norm 6 Use the workspace icon to When adding the data into the project or saving the line scan rtl file format the point spectra for each point in the line scan can be added to the Project by confirming the pop up window Do you want to save point spectra too a Save the line scan Use rtl fi...

Страница 101: ...il bar icon to Add Line scan to report Highlight elements in profile thumbnails Select Individual element profiles to add separate profiles for each element Select Composite element profile to show all selected elements in one diagram Fig 5 16 1 Quantitative line scan ...

Страница 102: ...manually by clicking the button One click terminates scan after finishing the last frame a second click terminates the measurement immediately 7 a map The processing of map data is described in section 5 19 8 Use the workspace icon to a Save Map data Use file format bcf to save HyperMaps datacube hyperspectral data set Spectra for each pixel are saved Further processing is possible only when data ...

Страница 103: ... or CRTL key b Add images to project Composite and individual element images will be added to Project c Add images to report Individual element images will be added to Report Alternatively click with the right mouse button into the thumbnail bar 11 Process Map data as desired Refer to section 5 19 For quantitative mapping see section 5 18 For phase analysis see section 5 20 optional license based ...

Страница 104: ...r to section 5 19 7 Use the tool to extract quantification results of regions of interest Quantification results appear in the Map result list 8 Click on to switch to pseudo colors display The pseudo colors display presents numerical quantification values Choose one element only for pseudo color display If several elements are selected the map displays summarized concentration values 9 Set Result ...

Страница 105: ...mages of selected thumbnails will be saved b Add images to project Composite and individual element images will be added to the Project c Add images to report Individual element images will be added to the Report Alternatively click with the right mouse button into the thumbnail bar Fig 5 18 1 Quantitative mapping ...

Страница 106: ...brightness gamma correction and color saturation e Map color mixing Use Enhanced to improve the display of EM image and element map overlay 5 Click on to switch to pseudo colors display Choose one element only for pseudo color display Right click on the icon to adjust Palette settings Note If the map is not quantified the values are normalized to the highest displayed intensity value 6 Extract poi...

Страница 107: ...rt icon in the Map tab to Save the map image Element selection Settings Result table Use image file formats bmp png jpg tif to save composite element image Alternatively click with the right mouse button into the map The options Add to project and Add to report are also available b Use the chart icon in the Charts tab to Save the charts image The options Add to project and Add to report are also a...

Страница 108: ...User Manual 5 Step by Step Guides 108 Fig 5 19 1 Map processing ...

Страница 109: ...open it Set parameters for phase determination 7 Select the AutoPhase Method All three AutoPhase methods work based on the number of element maps chosen Neighboring pixels containing the same chemical information represent a particular phase Depending on the chosen sensitivity pixels with similar composition get merged into one phase i PCA PCA Principal Component Analysis is a specific type of vec...

Страница 110: ... be merged into a single phase by highlighting the particular phases in the clipboard press CTRL or SHIFT key to highlight multiple thumbnails and pressing the icon b Extract a spectrum of a highlighted phase using the icon The spectrum will be displayed in the Spectrum tab 12 Use the workspace icon to a Save Map data Save datacube Hypermap as bcf file or map data as rtm file b Add data to project...

Страница 111: ...5 20 Phase Analysis QUANTAX EDS 111 Fig 5 20 1 Performing phase analysis ...

Страница 112: ...eport configurator to open the Report The Report preview Report is either docked to the right side of the screen or to the configurator bar The display can be changed using the icon in the Project tool 4 Edit review the report a Use Zoom to set display b Use Properties to set object layer order Objects are displayed as layers Uncheck Fixed when moving an object Check Pass on to show object on ever...

Страница 113: ...5 21 Creating a Report QUANTAX EDS 113 Fig 5 21 1 Creating a report ...

Страница 114: ...ght click into the image chart or result chart and use the local menu 3c Use the thumbnail bar icon and select Add to project Available in the Mapping workspace 3d Drag and drop an item from the current workspace chart to the Project The item appears in the Project list 3e Use the Project icon to Import an item from the hard disk Use the icon to toggle the position of Project It is either docked t...

Страница 115: ...ally saved to the hard disk Save the project file manually to archive your data Do not use Project to store HyperMap data The current map display can be added to the project but not the HyperMap data point spectra HyperMaps should be saved as described in 5 17 Fig 5 22 1 Creating a project ...

Страница 116: ......

Страница 117: ...20 36 Copy to clipboard 39 D Data Backing up 21 File formats 39 Load file 39 Loading 39 Save file 39 Saving 39 Transfer of SEM 17 Datacube 102 106 Dead time 16 Delete User 27 Detector Broken window 10 20 Window 20 Device settings 42 Display settings 43 Drift correction 59 Dwell time 34 E EBSD 28 Electromagnetic interference 11 Electron beam Deflection 17 Electron transparent samples Cliff Lorimer ...

Страница 118: ...gy setting 36 Maximum cooling detector setting 20 36 Method editor 81 Microscope configuration 33 Multi channel analyzer 15 Multi user systems 25 O Objects 28 Online manual 47 Option panels 30 P Phase analysis 109 Photon counting 15 Position tagged spectrometry 17 Preamplifier 15 Product license 42 Project File 39 Managing 114 Project tool 38 Projects 39 Pulse throughput 16 Q Quantification Bulk s...

Страница 119: ...ibration 45 Standard based quantification 88 Standardless quantification 83 Standards library 88 Bulk samples 73 Cliff Lorimer factors 76 Zeta factors 78 Standby 19 36 Stress sample 34 Supply voltage 10 Switch Box scan 17 System Assignments 41 Control panels 29 Report 41 Settings 41 Workspace 41 System Factor Calibration 70 T Thermostat mode detector setting 20 36 Twain export 39 U USB Dongle 19 U...

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