Laser, vacuum and gas reaction chamber for operando measurements at NSLS-II’s 28-ID-2

We present a laser reaction chamber that we have developed for in situ/operando X‐ray diffraction measurements at the NSLS‐II 28‐ID‐2 X‐ray powder diffraction beamline. This chamber allows for rapid and dynamic sample heating under specialized gas environments, spanning ambient conditions down to vacuum pressures. We demonstrate the capabilities of this setup through two applications: laser‐driven heating in polycrystalline iron oxide and in single‐crystal WTe2. Our measurements reveal the ability to resolve chemical reaction kinetics over minutes with 1 s time resolution. This setup advances opportunities for in situ/operando X‐ray diffraction studies of both bulk and single‐crystal materials.