Gas-controlled capillary spinner for time-resolved powder X-ray diffraction under dynamic conditions

Area of Science:

• Materials Science
• Crystallography
• Chemical Engineering

Background:

• Time-resolved X-ray diffraction (XRD) is crucial for understanding dynamic material processes.
• Controlling sample environments, especially gas atmospheres, is challenging for rapid measurements.
• Existing methods often lack the speed and environmental control needed for operando studies.

Purpose of the Study:

• To develop a novel gas-controlled capillary spinner for time-resolved powder XRD.
• To enable in situ and operando studies under dynamic and controlled gas atmospheres.
• To achieve high time resolution for tracking rapid structural changes in crystalline materials.

Main Methods:

• Integration of a gas-tight capillary cell, magnetic fluid rotary feedthrough, and fast-response diaphragm valve.
• Development of a system for continuous sample rotation with simultaneous gas control.
• Utilizing powder X-ray diffraction for structural analysis under varying gas conditions.

Main Results:

• The system demonstrated high performance with a standard Si powder sample, achieving <1% intensity fluctuations at ~200 rpm.
• Millisecond-scale measurements were successfully performed, showing improved diffraction peak uniformity.
• Time-resolved measurements of a metal-organic framework during gas adsorption tracked structural changes with 50 ms resolution.

Conclusions:

• The developed gas-controlled capillary spinner is a reliable tool for advanced in situ and operando XRD studies.
• The system facilitates the investigation of crystalline materials under dynamic gas environments.
• This technology enables quantitative analysis of rapid structural transformations during gas-solid interactions.