Attachment 1 SOW.pdf

Attachment 1- Statement of Work

TITLE: X-ray Diffraction System April 17, 2023

I. BACKGROUND INFORMATION

The National Institute of Standards & Technology (NIST) is issuing this solicitation for the purchase of an X-Ray Diffraction (XRD) system for the NanoFab multi-user facility in the Center for Nanoscale Science and Technology (CNST) in Gaithersburg, Maryland. The system will be sited and used as a shared resource in the NanoFab Cleanroom User Facility which is accessible to researchers from industry, academia, NIST, and other government agencies. The XRD will support nanofabrication research and development through the characterization of thin films and other materials by x-ray diffraction.

The NanoFab currently operates a Rigaku SmartLab x-ray diffraction system, originally purchased 2012, that is used to characterize a wide variety of thin film samples as well as powders and bulk samples. The new XRD is intended to replace the currently used Rigaku SmartLab X-ray Diffraction system before it reaches end of life and the associated problems.

II. OBJECTIVE

The CNST NanoFab intends to procure an X-Ray Diffraction (XRD) system that is a fully automated and a modular system for advanced x-ray diffraction measurements on a wide range of materials including thin films, bulk materials, and powders. The NanoFab is looking for an XRD system to replace the existing XRD capabilities which include powder diffraction, out-of-plane and in-plane thin film diffraction, reflection small angle x-ray scattering (SAXS), out-of-plane and in-plane texture, residual stress, rocking curves, and reciprocal space maps, on a wide variety of sample types (powder, bulk, ultra-thin to thick films, nano-materials, metals, and polymers). The x-ray diffraction system is housed in the NanoFab user facility, therefore ease of use in operation, system reconfiguration, and overall automation is paramount for low, medium, and high-resolution measurements. The system shall be able to run in manual and automatic modes.

III. MINIMUM REQUIREMENTS

The system shall meet or exceed the minimum requirements identified below. Preference will be given to systems that exceed the minimum requirements. All items must be new. Used or remanufactured equipment will not be considered for award. Experimental or prototype will not be considered. The use of “gray market” components not authorized for sale in the U.S. by the proposer are not acceptable.

The contractor shall provide a firm fixed price (FFP) quotation for the following:

CLIN 0001: Quantity one (1) X-Ray Diffractometer System for powder diffraction, out-of-plane and in-plane thin film diffraction, reflection small angle x-ray scattering (SAXS), out-of-plane and in-plane texture, residual stress, rocking curves, and reciprocal space maps, on a wide variety of sample types (powder, bulk, ultra-thin to thick films, nano-materials, metals, and polymers). Most of the measurements will be on blanket films where line focus illumination is preferred. The instrument shall be able to perform and record the auto test/alignment scans to assess alignment and tool parameters after a change of optics to help maintain a record of the instrument performance, measurement precision determination, and troubleshooting any improper instrument configuration.

The XRD shall meet or exceed the following minimum specifications listed below.

1. X-Ray Source A high flux rotating anode X-ray generator is required for measurements such as trace impurity material measurements, thin film measurements, micro-area measurement, small angle scattering measurements. The high intensity rotating anode x-ray source shall be mounted to the source goniometer arm of the theta-theta goniometer. The tube head shall scan in theta-source axis about the sample which remains horizontal during measurement for out-of-plane and in-plane diffraction conditions. A single electromagnetic shutter and interlock mechanism shall be included with the x-ray source.

a. Power: Minimum 5 kW continuous rated maximum output power

b. Target: Cu target anode, direct-drive/rotating anode

c. Vacuum: Turbo molecular vacuum pump (TMP)

d. Filament: Factory aligned and pre-mounted in cassette cartridge

e. Operation: Computer-controlled and manual operation

f. Safety Features:

i. Abnormal cooling water flow and pressure detection

ii. Abnormal generator overload detection

iii. Abnormal tube voltage detection

iv. Emergency stop switch

v. Leak current breaker

vi. X-rays completely shut off if any fail-safe devices are tripped or fail to operate.

g. Cathode Assembly, set up for line focus

h. One spare Cu anode shall be included

i. Set of 3 filaments included

The PRIMARY specifications listed above (a-h) are minimum specifications. A quoted system must meet or exceed all of these to be considered for award.

Stronger consideration will be given to an X-Ray Generator which meets the following SECONDARY specifications (j-o):

j. Focus: line focus preferred for Blanket films; 0.3 X 3 mm minimum

k. Voltage: 20kV – to at least 40 kV, move in 1 kV steps

l. Current: 10 mA – to at least 100 mA, move in 1 mA steps

m. Output Stability:< 1 % fluctuations, voltage and current

n. Preference is given to the system that allows the user to switch from out-of-plane to in-plane without changing from line to point focus optics, without changing the orientation of the source and sample relative to the detector, and without any realignment of the system.

o. Line focus is the preferred method for both out-of-plane and in-plane diffraction methods.

2. Radiation Enclosure and Chiller:

a. Radiation Enclosure: Steel construction with integrated lead panel direct beam stop, sliding door access, and lighted interior with viewing window(s).

b. Radiation enclosure shall meet all State and Federal Regulations.

c. Chiller: A refrigerated, water-cooled, or air-cooled chiller with capacity sufficient to cool the x-ray source continuously.

The PRIMARY specifications listed above (a-c) are minimum specifications. A quoted

3. 5-Axis High Resolution Goniometer with Eulerian Cradle, XYZ Sample Stage

a. Geometry: Vertical θ/θ goniometer with horizontal sample mounting and measurement

b. Capable of triple axis measurements

c. optical encoder controlled primary axes (θ, 2θ) d 5 Axes: ω, χ, φ, 2θ, 2θχ

e. Scanning Method: θs/θd independent or coupled

f. fully automated alignment

g. The 5-axis theta-theta goniometer shall include the ability to move the x-ray source in θs (also referred to as ω), the sample in χ and φ, and the detector in both 2θ (out-of-plane) and 2θχ (in-plane). 2θ and 2θχ detector scan axes shall be coupled to allow movement of the detector to any arbitrary position in reciprocal space substantially increasing the available range of reciprocal space for thin film measurements without needing to remount the sample and providing the ability to collect a whole pole figure by in-plane texture method. The sample stage shall provide ability for XYZ movement of the sample(s) and RxRy tilts for in-plane measurements where the surface normal of a sample shall be automatically oriented to the sample in-plane rotation axis. The sample stage shall provide fully automatic sample height alignment before each measurement and not require any manual height alignment of the system.

The PRIMARY specifications listed above (a-g) are minimum specifications. A quoted

Stronger consideration will be given to a 5-Axis High Resolution Goniometer with Eulerian Cradle, XYZ Sample Stage which meets the following SECONDARY specifications (h-o):

h. Sample Tilt: Minimum of χ = -5 to 95°, 0.001° minimum step

i. Sample Rotation: Minimum of φ = 0 to 360°, 0.02° minimum step

j. Sample Height: Minimum of Z = -1 to 1 mm, 0.05mm minimum step

k. XY Sample Stage: Minimum of XY = -40 to +40 mm, 0.05mm minimum step (6,400 mm2 mappable area) with the ability to hold up to 200mm wafer

l. Measuring Range:

i. Minimum of -3° ~ 160° 2θ reflection mode;

ii. Minimum of -80° ~ 160° 2θ transmission mode

m. Minimum Step Resolution (θ, 2θ): Minimum of 0.001° , Uncertainty for theta and 2 theta +/-0.05 degrees

n. In-plane Sample Tilt Stage:

i. Minimum of X Tilt = -5 to 5°, 0.01° minimum step

ii. Minimum of Y Tilt = -5 to 5°, 0.01° minimum step

o. In-plane Scanning Arm:

ii. in plane rotatin axis between = -3 to 100° with a minimum step of

0.04 degrees

4. Optics:

The XRD system must include both Bragg-Brentano (BB) and Parallel Beam (PB) optics for symmetric and asymmetric scanning geometries.

a. Optics:

i. Parallel Beam Optics with Multilayer X-ray Mirror

ii. Bragg-Brentano focusing Optics

b. Divergence Slit:

i. Computer-Controlled, Automatic Variable Divergence Slit.

ii. Divergence slit shall operate in fixed or continuously variable modes.

c. The incident optical system shall include both Bragg-Brentano (BB) and Parallel

Beam (PB) optics with a parabolic multilayer x-ray mirror. A method for switching from BB and PB optics quickly, easily, and without any manual realignment is necessary for the multi-user environment. The PB optics shall allow the user to easily change from slit collimation to choose of a Ge(220) 2-bounce, a Ge(220) 4-bounce, or Ge (400) 2-bounce channel-cut optics, as desired, without any manual realignment.

d. The goniometer shall have the ability to automatically align the optics and downstream optical path elements for use with a variety of Ge channel-cut optics (2-bounce and 4-bounce) to vary the resolution as needed.

The PRIMARY specifications listed above (a-d) are minimum specifications. A quoted

Stronger consideration will be given to an Incident Beam Optical System which meets the following SECONDARY specifications (e-j):

e. Simultaneously mounted, simultaneously aligned and user selectable parallel beam and Bragg-Brentano optical methods without mount and dismounting the parabolic multilayer x-ray mirror from the system and without any realignment.

f. The automated alignments of the source and optics shall be saved and printable for monitoring performance.

g. Incident Monochromators:

i. Ge (220) 2-bounce channel cut monochromator with 32 arc second resolution or better

ii. Ge (220) 4-bounce channel-cut monochromator with 12 arc second resolution or better

iii. Ge (400) 2-bounce channel-cut monochromator with 8 arc second resolution or better

h. Divergence Slit: Minimum of 0.05 mm ~ 7 mm, 0.01 mm step

i. Length of Illumination Area, Incident Height Slit: Minimum of 2.0, 5.0, 10.0 mm

j. Soller Slits:

i. Minimum Axial Divergence Angle 5° incident and diffracted beam for Bragg-Brentano

ii. Minimum Angular Divergence Angle 0.5° for Parallel Beam in-plane diffraction collimation

5. Diffracted Beam Optical System

a. Receiving Slit 1: Computer-Controlled Automatic Variable Anti-Scatter Slit

b. Receiving Slit 2: Computer-Controlled Automatic Variable Receiving Slit

c. Diffracted Beam Monochromator:

i. Curved Graphite for Bragg-Brentano

ii. Flat Graphite for Parallel Beam

d. Analyzer: Ge (220) 2- analyzer

e. The diffracted beam optics shall include dual receiving slit collimation, Soller slits appropriate for Bragg-Brentano and Parallel Beam (out-of-plane and in-plane methods), curved and flat graphite crystal monochromator, and Ge(220) 2-bounce analyzer. All diffracted beam optics shall have the ability to be switched quickly, easily, and without any realignment. The diffracted beam optics shall allow the user to easily change from slit collimation to Ge (220) 2-bounce analyzer without any manual realignment. The goniometer shall be capable of automatically aligning the optics and full optical path. The dual receiving slit shall be very well mechanically aligned in such a way that a knife edge collimator is not required for x-ray reflectivity measurements.

The PRIMARY specifications listed above (a-e) are minimum specifications. A quoted

Stronger consideration will be given to a Diffracted Beam Optical System which meets the following SECONDARY specifications (f-h):

f. Receiving Slit 1 Width range: 0.05 mm - 20 mm, 0.01 mm step

g. Soller Slits:

i. Minimum Axial Divergence Angle 5° for Bragg-Brentano

ii. Minimum Receiving Angular Resolution 0.5° for Parallel Beam

(out-of plane and in-plane methods)

h. Receiving Slit 2 Width range: 0.05 mm - 20 mm, 0.01 mm step

6. Micro Area Measurement Package

The system shall include a micro area measurement package to measure down to a 100 micron analysis area on the sample with high intensity. The micro area package shall include the following, at a minimum:

a. Optic which has the ability to convert a line focus source from the graded parabolic mirror into a high intensity point focus (100 microns or less) and allowing for automatic alignment. The beam on the sample shall be slightly converging and monochromatic (same energy filtering as PB configuration).

b. 0.05 mm and 0.1 mm collimators

c. Sample holder for micro spot diffraction

d. CCD camera sample positioning and viewing with auto focus

e. Image display on computer screen (<0.004 mm/pixel)

f. Mapping conditions available when combined with XY stages

7. Detector:

A multidimensional semiconductor, hybrid photon counting technology, detector with 0D, 1D and 2D measurement modes shall be provided. The detector must be able to be used for all applications and be able to operate in 0D, 1D, and 2D modes with minimal reconfiguration of the system. The detector must be able to easily switch between 0D and 1D modes by only software selection with no changes to hardware or optics. The detector must be able to easily switch between 0D/1D and 2D modes without removing the detector from the system. The detector must be able to be positioned from at least 150mm – 300mm from the sample when in 2D mode with detector distance being measured automatically by the x-ray system. Largest aperture required for wide range reciprocal space mapping by 2D detector mode and fast reciprocal space mapping by 1D mode using the same detector. The detector shall be suitable for Cu and Mo radiation.

The minimum Detector specifications:

a. Active area: 2900 mm2 or larger

b. Minimum Number of Pixels 250,000

c. Pixel size: 100 um x 100 um or smaller.

d. Background 0.1 cps or less (cosmic ray limited)

e. Maximum count rate: >1 x 106 cps/pixel

f. Efficiency for Cu Ka > 90%

g. Suppresses fluorescence

h. Can be mounted horizontally and vertically for max range of 2 theta coverage. Include hardware for mounting both ways

i. Shutterless operation, preferred no absorber required

j. Energy resolution 15%

The PRIMARY specifications listed above (a-j) are minimum specifications. A quoted system must meet or exceed all of these to be considered for award.

Stronger consideration will be given to a 2 D Detector which meets the following SECONDARY specifications (k-p):

k. Photon counting with global count rate 1.0 X 1011 cps

l. Incorporation of 2D continuous scan modes for fast reciprocal space mapping

m. Detector pre-configured for use with Cu, Mo source radiations

n. Server PC and associated software and hardware

o. Beam shaping slits

p. Includes horizontal and vertical mounting hardware

8. Small Angle X-ray Scattering (SAXS) Optics The theta-theta XRD system shall be able to be switched from wide angle to SAXS optics rapidly without any realignment and, if possible, without handling the x-ray mirror. The SAXS optical system shall use a line source with a parallel beam from the x-ray mirror with high resolution SAXS slit and automatically aligned parasitic scattering slit before the sample. No knife collimator shall be required. The SAXS optical system shall provide up to 100nm resolution on a conventional theta-theta goniometer. Sample stage shall be provided for both transmission SAXS of bulk, powder, or solution samples and reflection GI (grazing incidence)-SAXS on films on substrates. For GI-SAXS, sample height shall be automatically aligned by the system without any manual intervention. A vacuum pass on the diffracted beam side is required to reduce air-scatter.

a. Optics: Parallel Beam, pin-hole geometry

i. 2D- SAXS optics

ii. 2D WAXS optics

iii. 2D Transmission Attachment

iv. Vacuum Path for 2D-SAXS

v. Direct beam stop module

vi. Film sample holder

vii. Phi Stage

b. SAXS Analysis Software - Software to provide size distribution functions of nano-scale pore/particles and correlation length functions for materials with density fluctuation based on the non-linear least squares curve fitting analysis of x-ray small angle scattering profiles. Features include:

i. Slit correction

ii. Pore/particles size distribution analysis using curve fitting-based distribution function in volume and number fractions.

iii. Pore/particle modes include spheres, plates, rods and core/shell models.

iv. Correlation length analysis.

v. Features for transmission and grazing incidence reflection modes.

vi. Three different methods for analysis: size distribution, correlation length and model free.

9. High Temperature Stage:

Existing Anton Paar DHS1100 hot stage that was used on a Smartlab shall be adapted for use on the new XRD system.

a. Provide hardware for connecting the Anton Paar hot stage for use on the new XRD system

b. Provide electronic components and software for using the hot stage on the x-ray diffraction system

10. Accessories: required The system shall be provided with the following accessories:

a. Basic sample holders for powder measurements and alignments

b. Sample spacers for up to a 3 mm thick sample

c. Sample spacers to accommodate samples from 3 to 12 mm in thickness

d. 4” wafer holder

e. 6” wafer holder

f. Si reference standard

g. Si wafer alignment standard

h. Ni K-beta filter

11. Computer:

A control computer shall be provided. Windows Brand Name or Equal based computer with enough computing power to handle the advanced analysis routines.

a. Intel Core i7 or better processor (Brand Name or Equal)

b. 32.0 GB RAM

c. 24” Flat Panel Display

d. 512 GB Hard drive or better

e. Keyboard, scroll mouse and pad

f. Microsoft Windows 10 PRO, 64-bit (Brand Name or Equal)

g. MS Office 2019 Home and Business (Brand Name or Equal)

h. Adobe Acrobat Standard DC (Brand Name or Equal)

12. Software:

A single software platform that integrates instrument control, user guidance, data collection and data analysis is preferred. The software is used for instrument control, system status and device configuration, as well as optical system configuration, and measuring conditions. The system can be run in fully automatic or manual mode for alignments through analysis. At minimum, the following software programs must be included for the following data collection and data analysis functions:

a. Intelligence based Instrument control, data collection, and automatic alignment program capable of hardware configuration settings, optical component recognition, suggesting and checking combination of hardware settings for the desired application, HV settings.

b. Full featured powder diffraction and general XRD data analysis software for analysis of diffraction patterns with a variety of display tools and functions, automatic data reduction of background removal.

c. Reciprocal space map analysis and display program

d. Pole figure data analysis

e. Rocking curve simulation and analysis software.

f. X-Ray Reflectivity (XRR) analysis and modeling software.

g. Data mapping software to display XY plot of XRR analysis results, XY plot of rocking curve analysis results, and XY plot of general XRD data analysis results with color display, editing, and exporting of mapping images.

h. 10 individual software licenses

13. Software Licenses: International Center for Defraction Data (ICDD) Database Software

(PDF4) Brand Name or Equal: total of 3 licenses for 3 years

14. Application Training – onsite

a. Applications training for 3-5 people

b. 3 days of training covering instrument operation, data reduction and data analysis

15. Warranty and Service

a. One (1) year warranty (to cover parts, labor, and travel) shall be included with the base instrument. The vendor shall repair or replace at its cost, any defective items without any additional cost to the government including travel, labor, parts, or any other expense.

b. Warranty start date is the date of site acceptance.

c. The warranty shall cover the entire system and include on-site, telephone, and e-mail support. The contractor shall respond to support requests from NIST within two (2) business days of the request.

d. The contractor shall perform preventative maintenance on the XRD instrument at least once during the one (1) year warranty period.

e. The warranty shall include software updates necessary for proper tool operation and accurate data analysis.

f. All costs including parts, labor, travel, and other expenses necessary to repair the system (including all Contractor supplied hardware) shall be borne solely by the contractor at no additional cost to the U.S. Government.

g. Additional four years preventative maintenance shall be supplied by the Contractor as detailed in CLIN 0002.

16. Delivery

a. Upon successful factory testing, the contractor shall be responsible for delivering the system NIST, building 215 loading dock.

b. The contractor shall provide personnel that pass required government background checks to be issued badges for work on site.

c. The contractor shall schedule all visits to NIST for US citizens or permanent residents with the TPOC at least 2 weeks before arriving at the site.

d. A visual inspection of the equipment will be performed by NIST upon delivery to identify surface defects or any form of indication that any equipment was damaged during transport to NIST. The Government shall have sole discretion to require repair or replacement of damaged and/or nonconforming supplies at no cost to the Government.

e. Vendor is responsible for tool startup, demonstration of specifications, and training including travel, labor, or any other expense. During tool startup, vendor is responsible for running qualification wafers, working with NIST engineer, to demonstrate process capability.

17. Installation The system shall be installed by the Contractor and meet contract specifications no later than two

(2) weeks after delivery. Installation, at a minimum, shall include (i) uncrating/unpackaging of all equipment, set-up, and connection of the system to all necessary utilities, gas lines, etc., and (ii) demonstration of all specifications. Onsite installation and demonstration shall be done at NIST, Gaithersburg, MD.

18. Acceptance

a. Factory Acceptance: Before shipping the system, the contractor shall provide the

Government a standard factory acceptance report demonstrating that the XRD Instrument performs according to the contractor’s standard factory acceptance test.

b. Site Acceptance: The Contractor shall conduct their standard site acceptance test on standard reference samples, e.g. on a silicon reference sample or Al2O3 reference sample. In addition, at the NIST site the Contractor shall acquire data on the XRD instrument on NIST-supplied test specimens including thin films and epitaxial layers. The specimens and the measurements required for acceptance are described in the table below. The data shall be required to demonstrate conformance with the performance specifications defined in the Minimum Requirements section of this document.

Sample Required Measurements for Site Acceptance Test

Al2O3 SRM 1976b or Si SRM 640 Run powder scan on one or more of the Standard Reference Materials (SRM)s across the 2 theta angular range to identify peaks documented with SEM certificates. Validate that vendor provided peak search can identify the SRMs composition, either Al2O3 or Si..

Nominally 6 nm HfO on Si Perform X-Ray Reflectometry (XRR) scan from 0 – 10 degrees in 2 theta at a 0.01 degree step width and analyze the measurement using vendor provided software to determine thickness with +/- 1 nm.

Achieve 6 order dynamic range using Ge 220x2 bounce incident beam monochromator from a one hour measurement.

Reciprocal space map for SRM 2000 Perform a Reciprocal Space Map (RSM) using an area detector to validate mapping capability of SiGe epitaxy and evaluate thickness and either Ge concentration or lattice strain using vendor provided fitting software to validate RSM mapping and analysis capability. Validate the instrument profile function of the Ge 220x2 bounce and Ge 220X4 bounce incident beam optics using the Si (004) peak width.

CLIN 0002: Four Years Preventative Maintenance, that covers parts and labor, preventive maintenance and emergency service which shall meet or exceed the following minimum specifications:

a. The service contract shall begin at the end of the warranty period.

b. The entire system including options shall be covered.

c. The Standard system parts and shipping, including chiller shall be covered.

d. All labor, travel and expenses shall be covered.

e. One anode rebuild per year, including parts, labor, and balancing.

f. One preventive maintenance per year and emergency service shall be covered with 72-hour on site response or best effort.

CLIN 1001: (OPTION 1) Trade-in of the existing Rigaku SmartLab (SN JD2932N)

The vendor shall provide NIST the trade-in option of an existing Rigaku SmartLab (SN JD2932N) that NIST can exercise at the time of award to provide additional value to the government.

CLIN 2001: (OPTION 2) Quantity One (1) Mo rotating anode and associated optics for PDFs that can be swapped with the Cu rotating anode and associated optics.

a. Mo rotating anode source

b. Graded parabolic mirror for Mo source

c. Software for PDFs

d. Capillary spinning stage

e. Calibration and installation

NIST can execute this option at any time within one (1) year after Site Acceptance.

DELIVERABLES

Factory acceptance testing for the instrument

One (1) factory acceptance report 52 Weeks After Receipt of Order

(ARO)

Delivery of XRD Instrument (CLIN 0001) including all hardware and software necessary for full operation with Four Years Preventative Maintenance (CLIN 0002).

One (1) 52 Weeks ARO

Manuals for the instrument One (1) electronic copy of a user manual describing the XRD operation.

Complete manuals for all third-party components shall be provided in the format that is available to the Contractor.

52 Weeks ARO (with delivery of instrument)

Installation of the instrument One (1) 58 Weeks ARO

Successful site acceptance testing

One (1) 60 Weeks ARO

Training of NIST personnel at NIST, Gaithersburg MA

Three days on-site training 62 Weeks ARO

OPTION: CLIN 2001

Mo rotating anode and associated optics

One (1)

Within one (1) year after Site Acceptance

IV. PLACE OF PERFORMANCE

All work shall be completed at the Contractor’s facility. Installation of the instrument and training shall be performed at the customer’s site, NIST, Gaithersburg, MD.

V. PERIOD OF PERFORMANCE

The period of performance for all CLIN 0001 is 62 weeks from receipt of award, (see Deliverables above), except for OPTION CLIN 2001 (Mo rotating anode and associated optics) which shall be delivered within one year after site acceptance if executed. The base warranty shall last one (1) year after site acceptance. Four Years Preventative Maintenance (CLIN 0002) last up to four (4) additional years.