Transmission in situ and operando high temperature X-ray powder diffraction in variable gaseous environments

Area of Science:

• Materials Science
• Analytical Chemistry
• Physics

Background:

• In situ and operando X-ray powder diffraction (XRD) are crucial for understanding material transformations under dynamic conditions.
• High-temperature and controlled gaseous environments are often required for accurate material characterization.
• Existing setups may have limitations in gas control, temperature range, or time resolution.

Purpose of the Study:

• To develop and present a novel device for time-resolved synchrotron-based in situ and operando X-ray powder diffraction.
• To enable measurements at elevated temperatures (up to 1000 °C) under precisely controlled gaseous environments.
• To facilitate the study of materials under reaction conditions relevant to catalysis, battery research, and materials synthesis.

Main Methods:

• A gas-tight capillary-in-capillary design for sample containment and gas delivery.
• Integration of thermal mass flow controllers for precise gas flow control and on-the-fly gas mixing.
• Utilizing an infrared heated, PID-controlled capillary furnace for temperatures up to 1000 °C.
• Synchrotron-based X-ray powder diffraction for time-resolved data acquisition.

Main Results:

• Successful implementation of a device capable of time-resolved in situ/operando XRD measurements.
• Demonstrated capability to maintain stable, controllable gaseous environments at temperatures up to 1000 °C.
• The capillary-in-capillary design ensures efficient gas flow over the sample for accurate diffraction data.

Conclusions:

• The developed device offers a versatile platform for advanced materials characterization under demanding conditions.
• This setup significantly enhances the ability to study dynamic processes in materials science.
• The system provides a robust solution for in situ and operando investigations using synchrotron XRD.