HI-RES_WAXS_DETECTOR SoR v3.pdf

STATEMENT OF REQUIREMENTS

High Spatial Resolution Wide-Angle X-Ray Scattering (WAXS) Detector System with High-Energy X-Ray Sensitivity for Upgraded Ultra-Small-Angle X-Ray

Scattering (USAXS) Facility

I. BACKGROUND

The Materials Measurement Science Division (MMSD) in the Material Measurement Laboratory (MML) at the National Institute of Standards and Technology (NIST) provides the measurement science, standards, and technology required to enable world-leading materials characterization in support of addressing measurement challenges in linking materials composition, structure and microstructure to materials properties and performance relevant to the nation’s needs in technology and industry. In this connection, MMSD’s Materials Structure and Data Group (MSDG) collaborates as a partner with staff at the Argonne National Laboratory (ANL) Advanced Photon Source (APS), the brightest high-energy X-ray synchrotron facility in the Western hemisphere, in the development of a (recently upgraded) world-class ultra-small-angle X-ray scattering (USAXS) facility now located at APS sector 12-ID, and its application to materials measurement science in support of the NIST MML MMSD MSDG mission. These include additive manufacturing (AM) of alloys, ceramics AM, carbon dioxide reduction (CDR) through direct air capture (DAC) and carbonation, and measurement reference materials development.

The USAXS facility actually encompasses ultra-small-angle X-ray scattering (USAXS), small-angle X-ray scattering (SAXS) and wide-angle X-ray scattering (WAXS) measurement modes to provide comprehensive microstructure and structure characterization of complex samples over length scales from sub-nanometer to several micrometers in less than 5 minutes. The APS, itself, is being upgraded by the US Department of Energy (DoE) to APS-U, providing smaller, better defined, and more coherent X-ray incident beams. This in turn has enabled a major upgrade of the USAXS facility, allowing more stable operation to higher X-ray energies and enabling characterization over an even larger microstructure scale range. While the USAXS and SAXS measurement modes of the USAXS facility have been upgraded to take advantage of the new opportunities afforded by the APS upgrade, it remains to replace the WAXS X-ray detector, which provides diffuse scattering and X-ray diffraction (XRD) structure information that complements the microstructure information provided by the USAXS and SAXS measurement modes. The existing WAXS detector has limited X-ray sensitivity when used at the higher X-ray energies now envisaged to study denser materials and for pressure/temperature/gas environments requiring more substantial window materials. The present detector also has limited pixel resolution (pixels too large) resulting in poor XRD peak profile representation for fitting/quantifying XRD peak intensities from unknown phases. The new detector needs to address both these issues while also providing a very low, stable background and must also allow absolute intensity calibration over a large linear dynamic intensity range.

All of these considerations are taken into account in the detailed specification requirements set out below.

II. MINIMUM TECHNICAL SPECIFICATIONS

The Contractor shall provide a complete, turnkey high-spatial-resolution (High- Res), low-background, area X-ray detector system for wide-angle X-ray scattering (WAXS), with high-energy X-ray detector efficiency, low background, and large linear dynamic range (referred to hereafter as “Detector System”), meeting or exceeding the following minimum specifications:

1. The Detector System shall consist of a 2D (area) X-ray detector, any cooling system necessary for operation, readout electronics, control computer, control software and associated cabling.

2. The Detector System’s sensitive area shall be greater than or equal to 150 mm horizontal x 35 mm vertical.

3. The combined area of insensitive pixels or otherwise insensitive regions within the Detector System area shall not exceed 1 % of the total area.

4. The Detector System must perform with its detector plane vertical, must operate without interruption when mounted on a moveable detector stage, and all connections must accommodate the detector being moved over a distance of 500 mm.

5. The Detector System shall have a 2D spatial resolution at least equivalent to the 2D spatial resolution achieved with a pixel size of less than or equal to 80 μm x 80 μm and a point spread function not extending over neighboring pixels.

6. To be compatible with the brilliance and brightness of the APS-U synchrotron X-ray beams, the Detector System shall be capable of registering a count rate per pixel of up to 1 x 107 s-1.

7. The background count rate per pixel, including that associated with readout noise or dark current, shall be less than 20 s-1, and should not vary with time in use or with operating temperature.

*The Government will give preference to a system that uses single photon counting capability (i.e., be sensitive to single X-ray photons) to provide minimal background (effectively zero electronic background) for detection of weak X-ray diffraction peaks.

8. The Detector System shall have a minimum linear dynamic range from the background count rate up to the maximum count rate per pixel of at least 16 bits

(65,536 : 1).

*The Government will give preference to a system that can provide an effective linear dynamic range from the background count rate up to the maximum count rate per pixel of 20 bits (1,048,576 : 1) or more for measurements where weak scattering or diffraction signal must be distinguishable from background over short counting times: ≈ 10 ms.

9. The framing rate of the Detector System shall be greater than or equal to 10 Hz.

*The Government will give preference to a system that has a readout time less than 10 ms (effective frame rate greater than 100 Hz). Continuous readout with dead time < 3 microseconds with < 0.5 % defective pixels.

10. The Detector System shall be rated for operation over the full synchrotron X-ray energy range of interest: 5 keV to 40 keV with an energy resolution of less than 2 keV, and it shall have a detector efficiency of at least 60 % at 30 keV.

11. The Detector System dimensions, excluding connectors and connections, shall be less than 300 mm wide x 100 mm high x 300 mm deep, and the mass of the unit shall not exceed 8 kg.

12. The Detector System unit shall be cooled by forced air or liquid (water/glycol mixture) but any cooling circuit shall be sealed with the detector unit connected to a separate cooling unit via flexible tubing of > 7m length.

Connections to the back of the detector unit, itself, together with wires and tubes, shall not extend by more than 50 mm in the depth direction.

13. Electronics and computer hardware and software for Detector System set-up and data buffering/readout/processing/storage, including data formats, must be compatible with the Experimental Physics and Industrial Control System (EPICS) – see https://epics-controls.org/, as implemented for beam line control at the APS (https://epics.anl.gov), including EPICS area detector driver support, with a standard external trigger/gate 5 V TTL capability for the Detector System also provided.

14. Operations and Maintenance (O+M) Manual giving full description of operating and maintenance procedures shall be included.

Installation: The Contractor is not required to provide installation.

Training: The Contractor is not required to provide training.

Warranty:

The Contractor shall provide, at a minimum, a one-year warranty for the Detector System. The warranty shall cover all parts, labor, and travel. The warranty shall https://epics-controls.org/ https://epics.anl.gov/ commence upon successful completion of delivery and government acceptance based on demonstration of all required specifications. The Contractor shall provide telephone and/or email support during normal business hours for any set-up or operational problems encountered during the warranty period.

III. DELIVERY

Delivery shall be F.o.B. Destination and shall occur not later than (NLT) 180 calendar days after receipt of order.

F.o.B. Destination means: The Contractor shall pack and mark the shipment in conformance with carrier requirements, deliver the shipment in good order and condition to the point of delivery specified in the order, be responsible for any loss of and/or damage to the goods occurring before receipt and acceptance of the shipment by the consignee at the delivery point specified in the order; and pay all charges to the specified point of delivery.

The Contractor shall deliver the Detector System to:

Dr. Jan Ilavsky, Physicist X-Ray Science Division Advanced Photon Source Argonne National Laboratory 9700 S. Cass Avenue, Bldg 433A002 Argonne, IL 60439, USA

Telephone: 630/252-0866

E-mail: ilavsky@anl.gov

The Contractor shall notify both the APS-ANL Point of Contact (PoC) and the NIST Subject Matter Expert (SME) prior to shipment.

IV. DELIVERABLES

Description Quantity Due Date High-Spatial-Resolution High-Energy WAXS X-Ray Detector System

One System

NLT 180 calendar days post award

For acceptance into the beam line at APS, drawings showing the detector modules and connections, and the electronic circuit layout (e.g., technical specs) together with the factory test results showing the

One Set NLT 180 calendar days post award mailto:ilavsky@anl.gov

Description Quantity Due Date system is functional.

Word or PDF files acceptable Hardcopy and electronic copy of O+M manual

One Set NLT 180 calendar days post award

V. ACCEPTANCE CRITERIA AND TESTING

An initial visual inspection of the Detector System will be performed by APS-ANL to identify surface defects or any form of indication that the system was damaged during transport to APS-ANL. The Government has sole discretion to require repair or replacement of any observed damage to the system detected during transport, at no cost to the Government.

The NIST SME will work with NIST's APS partners to set up and incorporate the new Detector System into the beam line.

In addition to the inspection/acceptance terms articulated in FAR 52.212-4(a), the Government, prior to acceptance, reserves the right to conduct performance tests and evaluations to verify the Detector System’s performance. Such tests and evaluations will be conducted onsite at APS-ANL within the environment that the instrumentation is to be operated. The Contractor has the right to be present during the tests and evaluations at the Contractor’s expense.

Acceptance testing will be conducted by APS-ANL/NIST to verify the Detector System conforms to all technical specifications #1-13 and achieves successful results, by performing typical X-ray measurements on known material samples, including calibration standards.

Final acceptance by the Government shall be granted after confirmation that the Detector System meets all minimum technical specifications defined in the Statement of Requirements (SoR), including achieving satisfactory performance test results.

Should any deficiencies be noted prior to final acceptance, the Contractor will be notified and provided the opportunity to correct all deficiencies, at their expense.

Since X-ray beam time will need to be arranged at APS for acceptance testing, a period of 30 calendar days following delivery of the Detector System to the APS will be required for conducting this activity.

VI. PERFORMANCE REQUIREMENT SUMMARY

Desired Output Performance

Standard Monitoring Method

High-Spatial Resolution High- Energy WAXS X-ray Detector System is compatible with the USAXS facility as described above.

At the conclusion of acceptance testing, the

Detector System demonstrates compliance with all minimum technical specifications and is fully operational.

The Government will conduct the acceptance tests specified in Section V and verify that the Detector System meets the manufacturer’s performance specifications.

VII. INVOICING / PAYMENT

The Contractor shall invoice in one aggregate sum after the Detector System has been accepted by NIST. Partial payments are not authorized. Advanced payment is not authorized.

The Contractor shall be paid in accordance with net 30-day payment terms upon receipt and acceptance of a proper invoice.

The Contractor shall be paid according to the following:

100% after verification the Detector System is operating to OEM specifications, and final acceptance by NIST.