EDS_EBSD_Specs.docx

Specifications for an X-ray energy dispersive spectroscopy (EDS) and electron back-scatter diffraction (EBSD) system

GENERAL

Below are specifications for an x-ray energy dispersive spectroscopy (EDS) and electron back-scatter diffraction (EBSD) components for a variable pressure, high resolution, field emission scanning electron microscope (FESEM). The FESEM is being purchased through a concurrent procurement. The contractor in this procurement shall work with the vendor contracted to supply the FESEM.

Item 1. (required) The contractor shall supply an Energy Dispersive X-ray Spectrometry system which shall include the following features and capabilities:

Item 1A. Detector

1. Shall include a Silicon Drift Detector (SDD), with an active collection area of at least 50 mm2.

2. The detector, and associated electronics, shall be capable of collecting 200,000 x-ray counts/sec or better.

3. The detector shall have an x-ray photon energy detection range of 100eV to 30kV or better.

4. The detector resolution shall be ≤ 128 eV FWHM at Mn Kα, ≤ 57eV FWHM at C Kα, and ≤ 65eV FWHM at F Kα, all at ≥ 25 input kcps.

5. Peak shift due to higher count rates shall not be greater than 1eV up to 100 kcps.

6. The detector specifications shall conform to ISO 15632:2012 specifying performance at productive count rates.

7. The detector shall have a peak-to-background performance of 10,000:1 or better, and must be able to detect and quantify soft x-rays down to and including Beryllium.

8. The ratio of the oxygen to silicon peaks (using a SiO2 sample) at 10KeV and 35 degree take off angle shall be at approximately 1:1.

9. The detector shall be thermoelectrically cooled (Peltier cooler).

10. Vendor shall provide installation and training for the detector system.

Item 1B. Computer and Software

1. The software shall allow for dedicated user profiles, with settings specific to each user.

2. The software shall allow for spot, line, and area scans (maps). It is highly preferred that drift correction functionality is included. It is highly preferred that the software allows for the visualization of both phase and element distribution using a single image.

3. Software shall include spectral imaging and the ability to export images, spectra, maps, linescans in multiple file formats and different user-selected settings.

4. Software should be capable of automatically correcting for pulse pile-up, i.e. there should be minimal sum peaks and escape peaks in the processed spectra.

5. Application software shall be included for x-ray spectra acquisition and analysis. Full qualitative and quantitative (both standardless and standard based) software shall be included with ZAF, Phi Rho Z, and thin film matrix correction algorithms.

6. Auto-id, overlap, background correction, and the confirmation of element id capability shall be included.

7. The EDS system shall provide for at least six user-selectable amp times to provide full control of count rate and resolution.

8. The EDS system shall be capable of setting the amplifier’s amp time automatically to the optimal efficiency for the active count rate.

9. The analyzer shall be capable of accepting input count rates in excess of 300 kcps with a throughput greater than 200 kcps.

10. It is preferable that the EDS functionality be integrated into SEM control software; at a minimum SEM software should allow EDS software to control the microscope (column parameters, stage control, and image collection).

11. The EDS system shall have the capability to accept signals from multiple imaging detectors (i.e., x-ray, secondary electron, back-scattered electron, etc.) and capture the image.

12. The pixel dwell times should be ≤ 10 µsec for automatic collection of element maps and auto-drift correction during acquisition. The EDS system should be able to provide high precision EDS quantitative composition analysis with 512x512 pixel map in < 30sec. The dwell time shall have a user selectable range from 1µs (or less) to over 50ms per pixel.

13. The system shall be capable of storing the full spectrum for each location in an area scan for subsequent analysis.

14. The EDS software shall run on a computer provided with the EDS system (separate from the SEM). The EDS computer shall include at least 8 GB of RAM and a 1 TB hard drive.

15. The software shall be compiled for, and execute on, the Microsoft Windows 7 (or later) operating system.

16. The software shall allow for automated large area mapping: multiple fields collected over large areas, and stitched together, with field alignment through an image correlation algorithm.

17. Vendor shall provide installation and training for the software suite. At least one additional license shall be provided for off-line processing.

18. It is highly desirable that all future software updates and upgrades be included for the life of the system.

Item 2. (Highly desired) The contractor shall supply an Electron Back-Scatter Diffraction (EBSD) system which shall include the following features and capabilities:

Item 2A. Detector (EBSD pattern acquisition camera)

1. The camera and mount shall be designed to interface and operate to maximum performance with the full SEM system capabilities.

2. Shall have a speed & indexing rate of up to 100Hz at a 99% hit rate on a Ni standard sample.

3. The pattern images shall have a maximum resolution of 1344x1024 or better.

4. The detector shall have at least 12 bit grayscale resolution and a QE ≥ 70%.

5. Shall be capable of operation at SEM beam energy of 5 kV and 100 pA or less for high sensitivity.

6. Shall provide angular resolution of 0.1 degrees or less.

7. Shall provide spatial resolution of 25 nm or less.

8. Camera shall be capable of providing read-out rates of at least 100 frames/second @ 8x8 binning.

9. The detector shall have computer controlled motorized insertion and retraction with a positioning accuracy of 0.1 mm. The camera in its retracted position shall not interfere with normal SEM operation. The camera in its extended position shall interfere as little as possible with normal SEM operation.

10. The camera shall be suitable for orientation mapping, phase identification, discrimination of materials with similar crystallographic lattice parameters, and strain analysis applications.

11. Integrated forescatter diode(s) (FSD) shall be available, with the ability to provide orientation, topographical and composition imaging.

12. The FSD shall be software controllable from within the main application and without any peripheral hardware control units.

13. The camera shall be capable of acquiring patterns simultaneously with an EDS system.

14. Vendor shall provide installation and training for the detector system.

Item 2B: Computer and pattern acquisition software

1. Shall have the capability to accept signals from multiple imaging detectors (i.e., x-ray, secondary electron, back-scattered electron, etc.) and capture the image.

2. Variable scan speeds for image collection shall be available from 1 μs dwell to 800 μs in 1 μs intervals with several quick selection options. The software shall provide capability to raster over a reduced area of the image.

3. The software shall be capable of performing automatic phase identification based on EDS data or user supplied composition data.

4. Software shall provide for the ability to optimize the pattern collected utilizing background correction, gain control, selectable binning, integration time, etc. which may be turned off to process camera data at full resolution.

5. The system shall be capable of storing the patterns for each location in the region of interest for subsequent analysis.

6. The system shall be capable of controlling the electron beam to directly collect, display, and process digital images, for use with manual and automated analyses.

7. The system shall provide for drift correction.

8. The system shall provide capabilities to collect and index EBSD patterns:

a. In a manual, point by point mode.

b. In an automated mode, for generating two dimensional orientation data sets.

9. The pattern acquisition software shall control the high resolution camera used for EBSD pattern acquisition, including integrated controls for exposure, black level, binning, and background subtraction.

10. The pattern acquisition software shall allow for dynamic background subtraction for variable sample conditions (over or under saturation, rough surfaces, fracture surfaces, as-deposited surfaces, multi-phase materials with varying pattern intensity).

11. The EBSD software shall run on the same Microsoft Windows (version 7 or later) based computer as the EDS system.

12. It is highly desirable that the EBSD and EDS systems be fully integrated and allow for simultaneous acquisition of EBSD patterns and EDS spectra, with EDS data utilized in the phase determination process.

13. Vendor shall provide installation and training for the software suite.

14. It is highly desirable that all future software updates and upgrades be included for the life of the system.

Item 2C: Materials and Crystal Files

1. The data collection software shall include an integrated material file editor for the purpose of creating and refining electron diffraction reference data files, to be used for indexing, and shall not rely on external or “third party” software(s) for this capability.

2. The editor shall be designed specifically for electron diffraction data, with the ability to interactively enter lattice constants, symmetry and atom positions, subsequently creating and saving material files containing unit cell parameters, space group, and EBSD reflector planes.

3. The editor shall be able to directly modify, in an interactive manner, previously created material files.

4. The data collection software shall be able to directly update reflector plane information in material files via drawing lines on Kikuchi patterns or alternatively selecting/deselecting any reflector from a list, in no particular order.

5. The editor shall include the ability to import PDF card information from the ICCD database (database to be purchased/licensed separately through ICDD) and automatically convert x-ray reflectors to those appropriate for electron diffraction.

6. The editor shall allow for rejection of low intensity reflectors.

7. An electron diffraction materials database of at least 250 compounds shall be provided with the system.

Item 2D: Hough transform

1. Shall include multiple Hough transform routines with sophisticated parameter optimization that is able to index all seven crystal systems efficiently.

2. Interactive, user-adjustable Hough peak detection parameters shall include, but not be limited to:

a. Min/max number of peaks

b. Peak symmetry and distance

c. Binned pattern size

d. Display

3. Hough space results shall be displayed, with selected peaks marked and their corresponding bands indicated with color-coded lines on the diffraction pattern.

4. Selecting an unmarked peak in Hough space shall interactively highlight corresponding band in pattern, and vice versa.

5. A dynamic estimation of Hough transform time and resultant quality based on selected parameters shall be provided.

6. The option to save Hough data for every point during automated data collection (mapping) shall be provided.

7. The system shall provide progressive and high resolution Hough transforms for processing of high resolution (at least 1344x1024) digital images. For calibration of the pattern center, the system shall provide:

a. The ability to completely calibrate by automatic Hough band identification, manual band identification and zone axis locations, using any known phase

b. The ability to do a fine adjustment to calibration in a single step or push of a button

8. The system shall be calibrated for all practical working distances, and shall be able to work at any working distance or detector insertion distance with no need to recalibrate.

9. An interactive collection mode shall be provided.

10. The system shall provide the following capabilities without the need to export/save data to a separate data analysis software:

a. Point and click data collection using SEM images collected by the software.

b. Index, record and display orientation information for multiple points, including Euler angles, {hkl}<uvw> and Rodrigues vector.

c. Display and update pole figures or inverse pole figures with selectable indices, symmetry and projection modes for all available phases.

d. Manual indexing techniques via hand-drawn band selection and zone axis locations shall be provided as an alternative to automated Hough indexing.

11. Indexing results shall include:

a. Identification of correct phase.

b. Numerical means of ranking and distinguishing candidate phases.

c. Numerical measure for confidence in the candidate phases.

d. Angular fit.

e. Fit d-space.

Item 2E: Automated Operation

1. The system shall be capable of automatically collecting and completely indexing data, with accuracy greater than 95%, at a rate of at least 40 EBSPs/second (144,000 patterns/hour), at full resolution, on a suitably prepared, single-phase sample.

2. The data collection software shall be capable of simultaneously collecting and saving the following information for every point in a data set:

a. x-y coordinates

b. orientation parameters

c. diffraction pattern quality factor

d. Hough data

e. confidence measure

f. Energy Dispersive Spectroscopy (EDS) x-ray data.

3. The data collection software shall be able merge two or more scans to create a single multiple scan data set.

4. Automated runs for linescans and maps shall be created from field of view, rectangular, elliptical, or freehand regions.

5. Multiple map scans may be set up utilizing different magnifications, different resolutions, with data stored to separate files.

6. The system shall provide a dynamic estimate of scan time based on scan area, step size, and image collection time.

7. The data collection software shall have the capability to add comments to a scan file.

8. Automated orientation scans shall be able to collect and store data utilizing a hexagonal grid pattern, square grid pattern, and line scan.

9. The system shall be able to index and discern between multiple phases within a scan.

10. The system shall be able to index all crystal systems and crystallographic point groups.

11. System shall be capable of overlaying a fitted EBSD pattern geometry on the measured pattern:

a. using line centers

b. using line widths

c. color coded to reflector plane family

12. For automated operation, the data collection software shall provide:

a. A captured SEM image showing the extent of scan completed and current sampling location.

b. Ability to display, in real time:

i. Current pattern, bands, Hough results and indexing solution

ii. Scan progress in points, time per point, estimated time remaining

iii. Updated pole figures or inverse pole figures with selectable indices, symmetry and projection modes for all available phases

iv. Crystal orientation information on the sample image

v. Wire frame display of the indexed crystal structure

c. Ability to save EBSD patterns based on user selected parameters.

d. An accelerated, variable density scan mode, for locating and tracking grain boundaries while mapping a sample.

e. Automated grain size distribution analysis without saving or exporting data to external software.

f. Automatic tilt-correction for scan data.

g. Automated pattern center tracking and correction.

13. Data collection software shall include simulation capabilities:

a. For viewing predicted Kikuchi bands for a given phase

b. For viewing crystal wireframe for a given phase

c. For viewing pole figures or inverse pole figures with selectable indices, symmetry and projection modes for all available phases

d. To automatically scan through entire range of crystal rotations and predict problem reflectors for indexing of a specified phase

Item 2F: EBSD Data analysis software

1. The vendor shall provide a comprehensive software package for the analysis of orientation imaging microscopy data.

2. One license for the data analysis software shall be provided for the system, and at least one stand-alone license shall also be provided.

3. The data collection software shall have the ability to view and process orientation data during acquisition.

4. The data analysis software shall include a broad range of maps, charts, plots, and interactive analysis tools, be able to simultaneous display and process multiple data sets, and be able to fully process hexagonally sampled data, without converting or resampling to other formats.

5. Noise reduction and clean up procedures shall be provided to correct for EBSPs that could not be indexed, or were incorrectly indexed, without systematic alteration of microstructure. Capabilities shall include, but not be limited to: grain dilation, neighbor orientation, and neighbor phase.

6. The data analysis software shall have the following capabilities for mapping data:

a. Maps shall allow a grayscale or a color scheme to be assigned to points in the scan based on user-selectable parameter(s) associated with each point.

b. Simultaneous/overlaid grayscale and color-coded maps.

c. The parameter(s) associated with a map shall be scalable:

i. to cover the full minimum to the maximum range of values

ii. to cover only a partial range of the parameter

iii. as a percentage of the range or as absolute values.

d. Maps shall provide for the ability to:

i. View interactive, phase specific unit cell simulation

ii. Record interactive data

iii. Add user notes

7. The data analysis software shall be capable of creating subsets of data from maps by:

a. Cropping, via user-selected areas drawn directly on map image

b. Using data highlighted according to user-defined parameter(s)

8. Available map types shall include:

a. Confidence measure

b. Crystal orientation

c. Detector signal

d. XEDS

e. Elastic modulus

f. Grain average confidence measure

g. Grain average image quality

h. Grain average misorientation

i. Grain average video signal

j. Grain orientation spread

k. Grain shape aspect ratio

l. Grain shape orientation

m. Grain size

n. Image quality

o. Inverse pole figure

p. Kernel average misorientation

q. Phase

r. Schmid factor

s. Strain view

t. Taylor factor

9. The data analysis software shall be capable of determining and drawing boundary lines on maps to differentiate measurement points.

a. Boundary lines shall have user-selectable widths and colors

b. Multiple boundary types and ranges can be drawn on one map

c. The system shall provide for the following parameters for determining boundaries:

i. Rotation angle

ii. Rotation axis

iii. Axis angle

iv. Grain

v. Phase

vi. Coincident Site Lattice (CSL)

vii. Grain Shape Ellipses

viii. Reconstructed straight boundaries from segmented boundaries prescribed by the measurement grid

10. The software shall provide the capability to allow individual data points (or boundaries between data points) to be plotted in a variety of representations

11. The software shall allow to ability to measure and display the local misorientation.

12. The software shall be able to plot the distributions of measured parameters. Available plot types shall include:

a. Axis/angle misorientations

b. Euler space

c. Inverse pole figure

d. Misorientation Distribution Function – MDF

e. Misorientation profile

f. Orientation Distribution Function – ODF

g. Pole figure

h. Pseudo rocking curve

i. Rodrigues misorientations

j. Rodrigues orientations

k. Texture and grain boundary

l. Texture fibers (e.g. Alpha FCC rolling, Beta FCC rolling, Tau FCC rolling, etc.)

m. Texture index

13. Data analysis software shall provide interactive highlighting to cross-correlate data between maps, charts and plot, where highlighting may be done:

a. By manually selecting any feature(s) of interest in any map, chart, or plot

b. By user-definable tolerances for any parameter at a point or feature on a map

14. Data analysis software shall provide ability to export a grain file in text format, where available data for export shall include: phi1, PHI, phi2, x, y, image quality, confidence measure, area, diameter, major, minor, and phase.

15. Data analysis software shall provide ability for all images to be saved as bitmaps, tiff, or jpeg files.

16. Data analysis software shall provide the ability to automatically merge multiple data sets

17. Data analysis software shall provide the ability to generate templates that can be used create consistent measurements and displays across multiple data sets.

Item 2G: EBSD specimen holder (option)

1. A specimen holder shall be provided that is pre-tilted such that no tilt adjustment is needed to move to the EBSD position in the system.