New synchrotron powder diffraction facility for long-duration experiments
At a Glance
Section titled âAt a Glanceâ| Metadata | Details |
|---|---|
| Publication Date | 2017-01-27 |
| Journal | Journal of Applied Crystallography |
| Authors | Claire A. Murray, Jonathan Potter, Sarah J. Day, Annabelle Baker, Stephen P. Thompson |
| Institutions | University of Manchester, Diamond Light Source |
| Citations | 38 |
| Analysis | Full AI Review Included |
6CCVD Technical Documentation & Analysis: Synchrotron Powder Diffraction Facility
Section titled â6CCVD Technical Documentation & Analysis: Synchrotron Powder Diffraction FacilityâExecutive Summary
Section titled âExecutive SummaryâThis research details the construction and commissioning of the worldâs first dedicated Synchrotron X-ray Powder Diffraction (SXPD) facility for Long-Duration Experiments (LDEs), requiring materials capable of maintaining structural integrity and high X-ray transparency under extreme, non-ambient conditions for periods spanning weeks to years.
| Parameter | Summary |
|---|---|
| Core Application | In situ monitoring of slow kinetic processes (e.g., corrosion, crystal growth, gas capture stability) using high-brightness X-ray beams. |
| Material Requirement | Ultra-high purity, thin, and mechanically robust X-ray windows for specialized sample cells (e.g., low-temperature, high-pressure gas cells). |
| Key Material Used | Diamond windows are essential for beam entrance/exit due to low Z number (minimal absorption) and superior mechanical strength under non-ambient conditions (e.g., 243 K, 1 bar SO2). |
| Operational Criteria | High-energy X-ray beam (25 keV default) and small beam size (100 x 100 to 500 x 500 ”m) necessitate precise, thin diamond components. |
| 6CCVD Value Proposition | 6CCVD specializes in providing custom, optical-grade Single Crystal Diamond (SCD) wafers and plates, polished to Ra < 1 nm, ideal for high-performance X-ray transmission windows and specialized cell components. |
| Customization Need | Sample cells require custom dimensions, precise thickness control (down to 0.1 ”m), and specialized metalization (e.g., Au, Ti/Pt/Au) for hermetic sealing and brazing into copper or stainless steel cell bodies. |
Technical Specifications
Section titled âTechnical SpecificationsâThe following parameters define the operational environment and material requirements for the LDE facility, directly impacting the specifications needed for X-ray transparent components.
| Parameter | Value | Unit | Context |
|---|---|---|---|
| Photon Energy (Default) | 25 | keV | Optimized for penetration and fast data acquisition. |
| Wavelength (Default) | 0.49466 (1) | Ă | Used for CeO2 standard calibration. |
| Beam Size at Sample | 100 x 100 to 500 x 500 | ”m | Requires small, precisely aligned windows. |
| Resolution (Transmission) | 10-3 to 10-4 | âd/d | Sufficient for phase development and structural changes. |
| Low-Temperature Cell Range | 260 to 285 (-13 to 12) | K (°C) | Required for in situ MgSO4-11H2O (meridianiite) formation study. |
| Gas Capture Environment | 423 (150) | K (°C) | Desolvation temperature for NOTT-300 MOF. |
| Gas Pressure (SO2) | 1 | bar | Used for long-term structural stability testing of MOF. |
| Detector Active Area | 430 x 430 | mm | Large Pixium detector used for fast 2D pattern capture. |
| Detector Z Translation | Up to 3000 | mm | Requires highly repeatable sample-to-detector distance (±8 ”m resolution). |
Key Methodologies
Section titled âKey MethodologiesâThe LDE facility design and experimental procedures rely on highly stable, automated components capable of operating reliably over extended periods.
- Transmission Powder Diffraction Geometry: Utilizes a fast, large-area detector (Pixium) to capture whole Debye-Scherrer rings on a timescale of seconds to minutes, requiring highly transparent sample windows.
- Non-Ambient Sample Environments: Specialized cells were designed to simulate extreme conditions, including:
- Low-temperature mineralization cells (copper block body, refrigerant coolant, diamond windows).
- Gas capillary cells for corrosive gas capture studies (e.g., SO2 loading).
- Automated Operation and Cycling: The facility is designed to run multiple experiments in parallel, with automated, scheduled time-slice access (e.g., weekly measurements) over months or years, demanding high mechanical repeatability (micrometer level) from all stages and robust sample cell integrity.
- Small Beam Requirement: To achieve high-quality data in transmission geometry, the incident X-ray beam is tightly collimated (100-500 ”m), necessitating precise alignment and small, high-purity windows.
- Long-Term Structural Monitoring: Experiments track subtle changes in lattice parameters (e.g., NOTT-300 MOF) over 17+ weeks, requiring exceptional stability and repeatability in the X-ray optics and sample environment.
6CCVD Solutions & Capabilities
Section titled â6CCVD Solutions & CapabilitiesâThe successful operation of the LDE facility, particularly in non-ambient environments, hinges on the quality and precision of the X-ray windows used in the sample cells. 6CCVD is uniquely positioned to supply the high-specification MPCVD diamond required for replicating and advancing this research.
Applicable Materials
Section titled âApplicable MaterialsâTo meet the demands for high X-ray transparency, mechanical robustness, and thermal stability in the specialized LDE sample cells, Optical Grade Single Crystal Diamond (SCD) is the optimal material choice.
| 6CCVD Material | Specification Match | Application in LDE Facility |
|---|---|---|
| Optical Grade SCD | High purity, low absorption coefficient, high thermal conductivity (ideal for low-temp cells). | X-ray windows for beam entrance and exit in low-temperature mineralization cells and high-pressure gas cells. |
| SCD Thickness Control | Available from 0.1 ”m up to 500 ”m. | Essential for minimizing X-ray absorption and scattering while maintaining mechanical integrity under pressure/vacuum. |
| Polishing (Ra < 1 nm) | Ultra-smooth surface finish. | Reduces surface scattering and ensures optimal performance for high-resolution diffraction studies. |
Customization Potential
Section titled âCustomization PotentialâThe LDE facility utilizes bespoke sample cells (Small, Medium, Large, Type-R, Type-T) requiring highly customized diamond components. 6CCVD offers comprehensive services to meet these exact engineering needs:
- Custom Dimensions and Shaping: 6CCVD can supply SCD plates and wafers in custom shapes and sizes, ensuring a perfect fit for the specialized cell bodies (e.g., the 5 mm deep x 25 mm diameter chamber mentioned in the Meridianiite study).
- Precision Thickness Control: We provide SCD windows with precise thickness tolerances down to the sub-micron level (0.1 ”m), critical for maximizing X-ray transmission at 25 keV while maintaining pressure resistance.
- Advanced Metalization Services: For hermetic sealing and brazing diamond windows into copper or stainless steel cell bodies (necessary for low-temperature or gas environments), 6CCVD offers in-house metalization stacks:
- Standard Stacks: Ti/Pt/Au, Ti/W/Au, or custom layers (e.g., Pt, Pd, Cu) tailored for specific brazing or bonding requirements.
- Large-Scale PCD Capability: While SCD is preferred for X-ray windows, 6CCVD can supply Polycrystalline Diamond (PCD) plates up to 125 mm in diameter, which may be suitable for larger, less resolution-critical components or heat spreaders within the LDE instrumentation.
Engineering Support
Section titled âEngineering SupportâThe successful implementation of long-duration experiments requires deep expertise in material science and non-ambient cell design.
- In-House PhD Team: 6CCVDâs engineering and scientific team can assist researchers in selecting the optimal diamond grade, thickness, and metalization scheme to maximize X-ray transmission and ensure long-term structural stability for similar high-energy physics and materials science projects.
- Application Focus: We provide expert consultation for projects involving:
- High-pressure/low-temperature X-ray cells.
- Corrosion and electrochemistry studies requiring chemically inert windows.
- High-throughput screening systems utilizing diamond heat spreaders or detectors.
Call to Action: For custom specifications or material consultation regarding high-performance X-ray windows, specialized cell components, or other MPCVD diamond needs, visit 6ccvd.com or contact our engineering team directly.
View Original Abstract
A new synchrotron X-ray powder diffraction instrument has been built and commissioned for long-duration experiments on beamline I11 at Diamond Light Source. The concept is unique, with design features to house multiple experiments running in parallel, in particular with specific stages for sample environments to study slow kinetic systems or processes. The instrument benefits from a high-brightness X-ray beam and a large area detector. Diffraction data from the commissioning work have shown that the objectives and criteria are met. Supported by two case studies, the results from months of measurements have demonstrated the viability of this large-scale instrument, which is the worldâs first dedicated facility for long-term studies (weeks to years) using synchrotron radiation.