Attch 1- Requirements and Specifications Doc.docx

Attachment 1: REQUIREMENTS AND SPECIFICATIONS DOCUMENT TITLE: Procurement of X-ray Diffractometer with Silver X-ray Source

BACKGROUND INFORMATION

The National Institute of Standards and Technology (NIST), Material Measurement Laboratory (MML), Materials Measurement Science Division (MMSD-643) requires an X-ray diffractometer instrument with a silver X-ray source and optimized for measuring X-ray total scattering to support several NIST’s projects requiring the understanding of the local atomic order in materials and in situ studies of material processes. These projects include AI-assisted synthesis of metal-organic framework materials, high-throughput design of high-entropy alloys, additive manufacturing of metals, and developing methods for determining the local structure of inorganic and hybrid materials.

A silver X-ray source produces X-rays with a wavelength of 0.56 Å (K-alpha), which allows for significantly larger values of momentum transfer and much deeper penetration of X-rays into inorganic materials compared to the more commonly used copper X-ray source (K-alpha at 1.54 Å). X-ray total scattering data includes Bragg peaks that reflect the average atomic arrangement, along with a diffuse background that provides information about correlated deviations from this average. Effective measurements of total scattering require optimizing the instrument to minimize any unwanted backgrounds. By performing a Fourier transformation of the total scattering signal, one can obtain an atomic pair distribution function (PDF). PDF analysis facilitates the determination of local and nanoscale atomic order. High-quality PDFs necessitate large momentum transfer values, which can be achieved using short-wavelength silver radiation. Additionally, the deeper penetration provided by the silver source enables in situ studies of material reactions, such as those recreated in electrochemical or gas cells.

SCOPE OF WORK

The contractor shall deliver to NIST the equipment as described in Section III. Specifications are detailed below.

The system must be compliant with the world's most stringent requirements related to machinery safety (e.g., protection against moving parts), X-ray safety, electrical safety, and electromagnetic compatibility.

At installation, the X-ray diffractometer instrument must pass a documented acceptance test based on an established instrument verification procedure, demonstrating proper instrument alignment at a level that is currently state-of-the-art in X-ray powder diffraction. All interchangeable components of the X-ray diffractometer instrument (system optics, x-ray source, detector, and sample stages) must pass a documented acceptance test based on an established instrument verification procedure, demonstrating proper instrument alignment at a level which is currently state-of-the-art in X-ray powder diffraction.

Instrument alignment must be equal to or better than ± 0.01° 2-theta over the whole angular range, and the relative intensities must be accurate within ± 10% over the 2-theta angular range from 5 degrees to 80 degrees. The first specification is based on the NIST standard reference material SRM 640c (or its successor) and the second on SRM 1976b (or its successor). The resolution (full width half maximum) must be at least 0.07 degrees 2-theta in the 2-theta range from 20 degrees to 40 degrees using the NIST standard reference material SRM 660a (or its successor).

I. SPECIFICATIONS

Minimum specifications

1) X-ray Generator:

a. Voltage and current settings must be continuously adjustable via software.

b. NIST has a power supply for input voltage conditioning already in place.

2) X-ray Source:

a. X-ray source shall be a conventional sealed x-ray tube.

b. X-ray source target shall be silver.

c. X-ray source housing must be able to accept other standard conventional X-ray tubes, made of glass or ceramic, that are available from third parties, including source targets for copper and molybdenum radiation.

3) X-ray Optics:

a. Optics enabling transmission and capillary measurements

b. Computer controlled divergent slit and anti-scatter slit assemblies (incident and receiving)

c. Collimators, beam stops, and equivalent capabilities for reducing parasitic background scattering on both incident and detector sides

4) Geometries must include:

a. Horizontal or vertical goniometer

b. Independently driven omega and 2theta circles

c. Optical encoding system for goniometer positioning and accuracy

i. Minimum step size 0.0001°

ii. Step size reproducibility +/- 0.0005°

d. Software control/interface of components to prevent hardware collisions.

5) Detector

a. 1D (line) detector with >40 % efficiency for silver radiation

i. Single-photon counting

ii. Dynamic range: >10,000,000 cps

iii. Pixel size: 60 mm

iv. Fast readout: <100 ms

v. Energy discrimination against fluorescence

6) The instrument must be configured with the following user-interchangeable sample stages, and stage exchange must be able to be performed by laboratory staff at NIST:

a. Sample holder for capillaries capable of sample spinning

b. Sample changer for capillaries

c. Sample holder for flat samples for transmission measurements

d. Tools for mounting and aligning capillary samples

7) Reproducible positioning of optics and stages "alignment-free exchange"

a. All system optics, X-ray sources, detectors, and sample stages must be exchangeable and alignment-free, with reconfiguration possible by the NIST users onsite at NIST.

b. Unrestricted access into instrument enclosure to facilitate exchange of x-ray tubes, sample stages and instrument optics.

c. The enclosure must have large tempered leaded glass windows.to allow high visibility of the sample and any add-on components.

8) Computer System for instrument control, data acquisition, processing and analysis.

Computer system shall have the following features:

a. Windows 11-based computer

b. 1 TB hard drive or larger

c. 24" LCD monitor or larger

d. Keyboard (wired) with keypad

e. Mouse (wired)

f. 16 GB RAM or larger

g. 1 Ethernet ports minimum

h. 4 USB 3.0 ports minimum

9) Data Display, Processing and Analysis

a. Intelligent software to recognize hardware components

i. to prevent hardware collisions

ii. to facilitate hardware configuration changes and alignments.

iii. to facilitate hardware alignments.

b. Full data collection and instrument control software, including capabilities for batch control of multiple samples.

c. Data analysis software as described below:

i. Comprehensive codes for instrument control, performance monitoring, data display, data manipulation, data processing and analysis, including peak search, indexing, and profile fitting

ii. Data import and export in multiple file formats such as GSAS-II and X-Y.

10) Safety Enclosure: The system must comply with all State and Federal requirements for X-ray safety. It must provide full radiation protection, including safety interlocks. The enclosure must also allow the goniometer to be highly visible and accessible through large tempered leaded glass windows.

11) 24-hour response time for problem inquiries by telephone or e-mail during the warranty and service/maintenance period.

Additional preferred capabilities:

a. Johansson monochromator Ag Ka1 radiation with step-motor computer-controlled adjustments

b. Sample changer for capillaries (>5 capillaries, capillary spinning)

c. Control of the sample changer is integrated in the instrument software

d. Options for varying temperature during pair-distribution function measurements in the temperature range from 85 K to 1773 K.

e. Detector efficiency >80 % with Ag radiation

f. Minimum 2theta coverage at fixed detector position: 15°

II. ACCEPTANCE REQUIREMENTS

After delivery and installation, the contractor shall perform acceptance testing as follows:

Testing after start-up will consist of demonstration of the individual instrument components and their appropriate use and performance for data collection, this includes demonstrating the accuracy of each peak position over the entire angular range is equal or better than +/- 0.01 degrees 2-theta, using the NIST standard reference material SRM 1976b (or its successor). The resolution (full width half maximum) must be 0.07 degrees 2-theta in the 2-theta range from 20 degrees to 40 degrees using the NIST standard reference material SRM 660a (or its successor).

This test will also be performed after the exchange and/or reconfiguration of “alignment-free” components to demonstrate reproducible calibration. Evaluation/acceptance after installation will occur by NIST staff after the vendor demonstrates the instrument meets all the vendor specifications in the Gaithersburg, MD, laboratory.

III. INSTALLATION

The contractor shall install the instrument at the NIST, Gaithersburg, MD campus as a fully functional system.

IV. WARRANTY

The Contractor shall provide at least a one (1) year warranty to include field service, travel, labor and parts that were required. The warranty will not start until acceptance of the x-ray diffractometer by the Government (refer to section VII of this statement of work).

V. TRAINING

The diffractometer shall be offered as a fully functional system, complete and installed, with on-site training at NIST for a minimum of two days provided by a qualified manufacturer's XRD application scientist.

VI. PERIOD OF PERFORMANCE

Delivery of equipment no later than 180 days After Receipt of Order (ARO); Installation and training completed within 210 days after ARO.

VII. PLACE OF PERFORMANCE

All work shall be completed at the Contractor’s facility. Installation of the instrument and training shall be accomplished at NIST, Gaithersburg, Maryland. Normal duty hours are Monday through Friday, 8:30 a.m. to 5:00 p.m. with the exception of Federal holidays.

VIII. DELIVERABLES

IX. ACCEPTANCE CRITERIA

The NIST Subject Matter Expert (SME) and Contracting Officer Representative (COR) will verify that all performance requirements are met.