04 - SEM_Minimum Requirements.docx

MINIMUM REQUIREMENTS FOR A

Scanning Electron Microscope System

2020 FEB 20

GENERAL

AFIT requires a scanning electron microscope (SEM) with the following component and analysis systems: cathodoluminescence (CL), energy dispersive spectroscopy (EDS), electron backscatter diffraction (EBSD), scanning transmission electron microscopy (STEM), backscatter electron (BE) imaging, low vacuum imaging, temperature controlled imaging (-270C to 300C), cryogenic cross-sectioning polishing, cryogenic in-situ cleaving, sputter head with metal deposition capabilities, environmental isolation suitcase interaction, particle analysis software, elemental mapping software, photo-emission (CL) mapping software, elemental analysis software, image montaging software, and image post-processing software.

This system is required for imaging and analysis of nuclear materials used in processing or post detonation nuclear blasts. Micro-analysis via SEM and accompanying sample preparation, detection, and analysis systems supports nuclear engineering, nuclear diagnostics, non-proliferation, radiation effects on electronics, radiation weapons effects, radiation detection, biological culture analysis, micro-electromechanical systems (MEMS) devices, nanomaterials and machine learning education and research; associated in with at least three departments of AFIT.

To accomplish these educational objectives, the SEM is required to have the specification list below. Of critical importance is image resolution with a minimum of 0.9nm at 20.0kV (WD 10mm, 5nA).

This specification list provides the minimum requirements for the XRF Microscope:

1. Accelerating voltage range 0.01 to 30.0kV

2. Beam current range 1pA to >300nA

3. Magnification range 10x to 1,000,000x (128x96 mm photo)

4. BE Detector similar to SM-84033SRBEW (Manufacturer: Jeol): Short working distance solid state backscatter electron detector with resolution of 1.5nm at 30kV or better

5. Shottky-type, in-the-lens, thermal field emission electron gun

6. Retractable low vacuum system

7. 5 axis motor drive stage (X,Y,Z,TILT,ROTATION)

8. Specimen exchange chamber

9. Stage navigation system

10. Hybrid chamber camera

11. Retractable backscattered electron (BE) detector

12. Retractable motorized annular STEM, HAADF/MAADF/LAADF/BF

13. Cathodoluminescence (CL) imaging spectrometer/detector

14. Energy dispersive spectroscopy (EDS) – Electron backscattered diffraction (EBSD)

15. Integrated functionality to include automated stitching/montaging for high resolution image acquisition across large areas that incorporates tilt correction, field overlap, and autofocus point setting

16. Integrated functionality to include creation of 3-D imaging

17. Environmental cell sample loader

18. CRYOGENIC PREPARATION SYSTEM: Similar to EMS-PP3010T (Manufacturer Electron Microscopy Sciences)

1. Gas cooled cold stage with integrated heaters and temperature sensor. Cold stage temperature variable down to -190°C or colder and up to 100°C or hotter with a stability < 0.5°C.

2. Gas cooled anti-contaminator (cold trap) and variable position mount, including temperature sensor capable of reaching -190°C or colder.

3. The cold stage and anti-contaminator cold trap must be cooled independently of each other via separate gas lines.

4. Cooling must be controlled via Electronic gas flow control valves equipped with flow sensors.

5. All feed-throughs, bellows, or flange adaptors for cold gas supply to the cold stage and anti-contamination cold trap, or specimen transfer must be performed by installer and included in price.

6. Any SEM stage adaptors must be installed by manufacturer or included if removable.

7. The cryogenic preparation chamber must be mounted directly onto the microscope using a suitable chamber port.

8. Pneumatic gate valves must be equipped with fail safe interlocks, and be fully integrated.

9. The cryogenic preparation chamber must have a large front window (150mm x 78mm or larger) plus two top viewing ports, as well as a CCD camera for the observation of specimen fracturing and pickup. The CCD image must be shown on the control panel PC.

10. The cryogenic preparation chamber must be fitted with a front mounted fracturing and manipulation device fitted with a #5 scalpel.

11. The cryogenic preparation chamber must have a micrometer advanced fracturing tool with a hardened steel blade.

12. Both fracturing devices must be actively cooled.

13. The cryogenic preparation chamber will be fitted with a fully integrated,, automatic, high resolution sputtering head including one platinum (Pt) and one chromium (Cr) target.

14. The cryogenic preparation chamber must be directly pumped through the back of the chamber.

15. The cryogenic preparation chamber must include a multi-range vacuum gauge fitted directly to the chamber.

16. The cryogenic preparation chamber must include multiple (more than 2) LED lamps focused on the specimen stage.

17. The cryogenic preparation chamber must include an interlocked gate valve to airlock with roughing line directly connected.

18. The cryogenic preparation chamber must include an opto-switch sensing of cryo transfer device being fitted to the chamber airlock.

19. The cryogenic preparation chamber must include a stand-alone turbo stack that pumps at 70L/s or greater with a base pressure < 1E-6 mbar.

20. The cryogenic preparation chamber must include liquid nitrogen slushing (freezing) and specimen manipulation with fully integrated power and control units.

21. The slushing process must allow for specimen tilting for manipulation and vacuum transfer of specimens.

22. The cryogenic preparation chamber must include a “parking tube” for cryo transfer device storage when not in use.

23. The cryogenic preparation chamber must provide a customizable interface and processes with user definable “recipes”

24. The cryogenic preparation chamber must allow on screen data logging and system diagnostics.

25. The cryogenic preparation chamber must provide a fully automated sputtering process.

26. The cryogenic preparation chamber must provide a fully automated sublimation process.

27. Any required specimen shuttles must be provided at the time of installation.

28. A minimum of 10 blank stubs (10mm) will be provided at the time of installation.

29. A minimum of 5 stubs with holes and slots (7mm) will be provided at the time of installation.

30. A minimum of 5 stubs with holes and slots (5mm) will be provided at the time of installation.

31. A minimum of 100 brass rivets for fracturing liquids will be provided at the time of installation.

32. A minimum of 5 copper (Cu) stubs with 3mm x 3mm slots will be provided at the time of installation.

33. A minimum of 5 copper (Cu) stubs with 1mm x 3mm slots will be provided at the time of installation.

34. Specimen mounting compounds (colloidal graphite and Tissue-Tek® will be provided at the time of installation

19. Plasma cleaner

1. Must include a portable controller with embedded microcomputer and LCD touchscreen user interface.

2. Must include a Remote plasma source (high quality quartz tube) with KF/NW40 vacuum interface.

3. Must include a 75 watt RF power supply or greater.

4. Must include a plasma strength sensor/monitor.

5. Must include an electronic gas dosing valve with pressure sensor feedback control.

6. Must include an automatic cleaning cycle.

7. Must include an NW40 adapter flange for SEM/FIB integration.

8. Must include at least 15 feet of high quality high power RF cabling, D-Sub 15 source control cable.

9. Must be capable of at least 60 user customizable recipes on the touchscreen controller.

20. Cooling cross section polisher

21. All pumps, chillers, computers, monitors, switch boxes, sub-system components and initial consumables required for proper installation and operation.

22. Compact in-line nitrogen gas dryer with built-in heater for adsorbent regeneration

23. HP Workstation Z440/CMT or equivalent with an Intel Xenon E5-1620V3 processor (3.50GHz) or better, 16GB Ram or better, 500GB Hard Drive or better, Super-multi drive, Windows® 10 Professional 64 bit (English) or newer, Ethernet (10/100/1000BaseT) x2, digital scan generator board and image acquisition/display board

24. Windows 10 Professional Operating System or newer

25. Image archiving and database management similar to Smile View™ Lab - a fully integrated data management software which links the CCD image, SEM images, EDS analysis results, and corresponding stage coordinates for fast report generation or re-call of sample position for further study. This data manager saves the data, which links the observation position, observation and analysis results, and a low magnification image acquired by Holder Graphic or CCD image. You can review or re-analyze already acquired data and export them to a report. Allows for a data search by specimen name, creation time, or data type.

26. Adjustable objective lens aperture strip

27. Aperture Angle Control lens (ACL)

28. Highly conical objective lens with through-the-lens (TTL) detection system

29. Chamber camera similar to JEOL Hybrid chamber camera SM-74330HCS (Manufacturer: Jeol)

30. Camera may not interfere with the performance of any detector (i.e. operator need not turn camera off during system operation in any mode, or camera should automatically turn itself off)

31. Conventional in-chamber E-T type Secondary Electron Detector

32. Upper electron detector with energy filter

33. Transmission Electron Detector similar to SM-14050RTED (Manufacturer: Jeol): Retractable scintillator based detector for imaging transmitted electron signal in SEM. Includes bright-field and dark-field imaging modes. Includes a specimen holder for 3mm TEM specimens.

34. Cathodoluminescence (CL) Detector similar to Centaurus CL & Backscattered Electron detector DEBEN-907-00012 (Manufacturer: DEBEN) (Document 2) with optional motorized insertion. Centaurus is a scintillation type backscattered electron or CL detector that can generate either compositional (with topographic information) BSE images or with a quickly removable tip, it can be converted to a CL imaging detector giving an additional function

35. Energy Dispersive Spectroscopy (EDS) silicon drift detector (SDD) similar to the EDAX Octane Elect Super EDS system PV5500-EL-SU-HSuper (manufacturer: EDAX) (Document 3a). This is a 70 mm2 chip made of Si3N4 suitable for low voltage (kV) microanalysis, and has mapping speeds greater than 400,000 output counts per second (cps). This detector must be suitable for use with corrosive and plasma cleaning environments.

36. Electron Backscattered Diffraction Spectroscopy (EBSD) detector similar to the Hikari Super EBSD Camera PV5500-EL-SU-HSuper (Manufacturer: EDAX) (Document 3b). This camera is capable of 1,400 indexed points per second, and comes with a Forward Scattered Detector and EDAX’s patented Pattern Region of Interest Analysis System (PRIAS™) software. It is capable of imaging utilizing beam currents as low as 100pA, and accelerating voltages as low as 5kV. It has angle orientation precision to less than 0.1 degrees.

37. The PRIAS™ software (Document 3f) is capable of providing 25 images from pre-defined regions of interest that can be arithmetically processed to enhance, suppress, or isolate specific image contrasts which is needed for microstructural analysis. It is further capable of synchronous imaging of orientation, phase, and topographic contrasts of EBSD samples.

38. User-selectable bias applied to the specimen for primary beam deceleration (operational at all kvs). This function reduces the impact of lens aberrations on the probe size, resulting in improved resolution, enhanced surface detail and charge reduction. Allows imaging down to 10V (i.e. 0.010kV).

39. Digital scan generator system with up to 5120x3840 pixel resolution by 8 bits. TIFF images can be acquired at 16 bit

40. Computer-Eucentric tilt compensation

41. More than 20 user selectable scan speeds

42. Frame averaging and integration

43. Charge free (CF) scan

44. Live signal mixing of up to 4 signals

45. Fully automatic and fail safe interlocks

46. Pneumatically controlled valving

47. Ion pumped UHV gun chamber and intermediate chamber

48. Ion pump battery backup system

49. Sample chamber pumped by TMP

50. Automated variable pressure (i.e. the control for switching vacuum modes must be fully integrated into the software operation)

51. Operating pressures between 10-300 Pa

52. Gas: dry N2

53. Imaging: BSE/LV-SE

54. Resolution: LVBED (30kV, 10Pa) – 1.8nm

55. 5-axis motor drive stage 86mm or larger fully integrated with STEM detector and heating/cooling stage

56. Particle Analysis software must provide Particle and phase analysis with comprehensive image analysis and chemical analysis designed to detect and chemically analyze particles, inclusions or phases from single or multiple EDS and SEM/STEM fields of view. The user must be able to define a gray level and particle size threshold and search for 12 or more morphometric parameters. The user must be able to define 8 or more phases by gray level to segment the data and particles to be analyzed using regions of interest data, net intensities, k-ratios, or by ZAF (atomic number absorption factor) weight % via irregular shape scale or particle centroid mode. Spectra must be saved for each particle or phase with the spectrum collected at the centroid or from the core of the particle with the percentage of the particle defined by the user.

A matrix of stage locations with a search resolution of 2048x1600 points per field or better must be capable of data collection while unattended with beam shut off at end of search. Analysis/searching may also be stopped when a specified number of particles/phases are found within a field, then analysis resumes on the next field. Particles on the border of a field must be indexed for exclusion or inclusion with the possibility to be revisited while viewing the image, particle data or spectrum.

Images must be capable of saving in BMP or TIF (uncompressed) file formats and the particle summary data including both morphometric and chemical data must be capable of being saved as a CSV file compatible with MS EXCEL and Matlab. A simple screen capture feature/tool must also be included for incorporation of additional graphical or equipment specific data.

At the conclusion of analysis, it must be possible to interrogate the particles or phases on the image for their relevant data and to view the spectrum for each particle. Particles must also be capable of being sorted on morphology or chemistry and spectra be quantified again at this time, or correlated via color-coded ternary plots. The software must have the capability of merging spectral data from various fields into a single directory.

57. EDS Spectrum Library: Similar to SPECTRUM MATCH PV6366-00 AND PV6066-00 (Developer EDAX)

PERIOD OF PERFORMANCE

The customer will receive all components 6 months after contract award.

DELIVERY AND TRAINING

The contractor will deliver hardware to the Air Force Institute of Technology (AFIT) at WPAFB, OH. Training will be provided once system has been installed, and certified for resolution requirements.

WARRANTY

JEOL manufactured equipment is guaranteed against defects in workmanship and component failure for a period of five years from the date of customer's first use of the instrument. In the event that installation and/or acceptance is delayed by the Customer but not by JEOL, the warranty period will begin 60 days after the agreed upon delivery date. Under this warranty policy the labor necessary to repair the instrument and all parts (except consumables) are provided by JEOL at no cost to the Customer. JEOL reserves the right to repair or replace components at their sole discretion. The warranty does not cover components which have been damaged through misuse or accident on the part of the buyer nor does it include components which have been modified by the customer.

PAYMENTS

90% Net 30 days after Delivery 10% Net 30 days after Acceptance Acceptable forms of payment include Check, Wire, or ACH