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

A gas-controlled capillary spinner was developed for time-resolved powder X-ray diffraction measurements of crystalline materials under controlled atmospheres. This system enables continuous sample rotation with simultaneous gas control by integrating a gas-tight capillary cell, a magnetic fluid rotary feedthrough and a fast-response diaphragm valve, allowing diffraction measurements to be performed in rapidly changing environments. The system performance was evaluated using a standard Si powder sample, revealing that high-speed rotation significantly improves the uniformity of the diffraction peak intensity, with relative fluctuations reduced to <1% at speeds of ∼200 r min-1 even with millisecond-scale measurements. The applicability of the system was demonstrated by time-resolved diffraction measurements of a metal-organic framework during gas adsorption, in which structural changes were successfully tracked and quantitatively analyzed with a time resolution of 50 ms. These findings indicate that the developed system provides a reliable approach for in situ and operando diffraction studies under dynamic gas conditions.