Appendix C - Specifications.pdf

Appendix C - Specifications dated 11/2024

Advanced X-ray powder diffraction system for the scientific investigation of intermetallic alloys, compounds, and thin films

List of requirements

Ames National Laboratory of the US Department of Energy is in need of a new multipurpose X-ray diffractometer (XRD) system suite with specific experimental capabilities that include 1) a high power and brilliance rotating anode X-ray source/generator, 2) Bragg-Brentano (BB) para-focusing, as well as parallel beam (PB) optics, 3) High resolution incident beam monochromator, 4) Helium cryostat non-ambient temperature stage, high temperature non-ambient stage, 5) Eulerian cradle for thin film measurements, 6) multidimensional (0D/1D/2D) X-ray detector with high energy capability.

Capability to perform i) measurements in applied magnetic field, and ii) automated multiple sample characterization is desired but not mandatory.

Specific Requirements:

High power & high brilliance rotating anode X-ray generator The main system X-ray generator should have high brilliance, fine focus, and at least 6 kW X-ray rating (9 kW preferred) using a Mo and/or Cu anode. This system must be usable effectively for such measurements as trace impurity material measurement, thin films and non-ambient temperature measurements, where the conventional sealed tube systems have difficulty producing sufficient intensity, and therefore signal. The rotating anode source should be manufactured and supported by the instrument manufacturer. The anode should be user serviceable for replacement. Replacement and refurbishment should be performed quickly by the instrument manufacturer to avoid downtime. A second anode is required to minimize downtime during maintenance. A water chiller system for cooling the anode must be included.

Bragg-Brentano Para-Focusing (BB) and Parallel Beam (PB) Optics

A high performance optics must be included, including the ability to convert a divergent beam into a parallel incident beam with a divergence of 0.04° or better. All components must be possible to align automatically. The XRD system must include both Bragg-Brentano (BB) and Parallel Beam (PB) optics which are user selectable on demand without ever removing the x-ray mirror or diffracted beam monochromator from the system and without any realignment. The X-ray optics should be manufactured and supported by the instrument manufacturer.

High Resolution Monochromator Ge (220) 2-Bounce Incident Beam Monochromator

Ge (220) 2-bounce high-resolution channel-cut incident beam monochromator for high-resolution parallel beam measurements of the crystal structure of imperfect materials. Fully automated channel cut Ge crystal must provide precise alignment and user-friendly operation.

Sample Stages:

All Sample stages include component recognition function, compatible with goniometer mounting and Z-control and include both automatic stage alignment and automatic sample alignment.

Closed Loop Cryostat

A closed cycle cryostat designed for cooling flat plate powder samples to temperatures as low as 12 K using fast and controllable cooling with no consumption of cryogens such as helium or nitrogen.

Temperature stability of 0.1 K, and fast cool down and warm up times (less than 1 hour) for easy access and sample change are preferred. Weight is less than 10 kg. Power 230V 50Hz or 100/115V 50/60Hz.

Includes helium compressor with cryostat, coldhead, controller, cryodrive, vacuum assembly with pump, software integration.

High Temperature Oven Chamber

High temperature attachment operating at temperatures from room temperature up to 1000°C or higher under vacuum with software integration. Vacuum pump included. Sample spinning capability included for capillary samples. Capillary extension allowing heating of samples inside glass capillaries required.

χ-φ-Z Eulerian Cradle

Eulerian cradle providing sample tilt and rotation axes to move sample in χ, φ and Z axes. High-precision motor driven sample stage, χ: - 5 ~ 95 º / 0.001 º step; φ: -360 ~ 360 º / 0.002 º step.

Automatic Sample Changer with Spinner

Automatic sample changer for reflection and transmission measurements. Integrated sample spinning improves particle statistics in polycrystalline sample measurements. Fully automatic alignment.

Programmable.

Capillary Stage Attachment

Automated sample stage for use with glass capillary tubes. Includes sample-spinning capability. Design in a way to simplify capillary alignment and provide precise positioning into the beam. Spinning: 1 – 120 rpm.

Detector:

Multidimensional (0D/1D/2D) Detector with High Energy capabilities

To serve a wide range of XRD experiments, a highly versatile multidimensional (0D/1D/2D) detector with a large active area is required. 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. High efficiency required for Mo radiation.

The detector must be manufactured by the X-ray system vendor to ensure long term software and hardware support, long term parts supply, continued software and hardware development to ensure future capabilities can be sourced, and seamless integration into vendor’s X-ray system software and hardware platform. The detector shall not require any maintenance including operating gases, gas recharges over its lifetime, or water or liquid nitrogen cooling. The detector must operate maintenance-free.

System Software:

At minimum, the following software programs must be included for the following data collection and data analysis functions:

1) 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.

2) 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,

3) Rocking curve simulation and analysis software.

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

5) 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.

6) The software should be manufactured and supported by the instrument manufacturer.

Computer:

Windows based computer with sufficient computing power to handle the advanced analysis routines, with at least a Microsoft Windows 11 PRO, 64-bit operating system, MS Office 2022 Home and Business, Adobe Acrobat Standard DC.

Training, Installation, & Warranty:

Full installation to include all functional system components and a demonstration of their full function must be included. A one-year full system parts and labor warranty, with full on-site service, must be provided on the system.

The system must include on-site training to be performed at the customer’s site for 3 days to cover diffraction physics, sample preparation, system operation, and data analysis.

Safety

The equipment must be compliant with Ames National Laboratory safety regulations and requirements.

Safety Features:

• X-ray “ON” warning light

• Abnormal cooling water flow, pressure and vacuum level detection

• Abnormal generator overload and tube voltage detection.

• Emergency stop switch.

• Leak current breaker.

• X-rays completely shut off if any of the fail-safe devices are tripped, or fail to operate.

Radiation Enclosure

• Steel construction with integrated lead panel direct beam stop.

• Safety interlocked with electromagnetic shutter mechanism.

• Sliding front access doors with high/low leaded-acrylic windows.

• Lighted interior.