Laser, Vacuum, and Gas Reaction Chamber for Operando Measurements at NSLS-II's 28-ID-2

TL;DR

This paper introduces a versatile laser reaction chamber enabling rapid, in-situ X-ray diffraction measurements under various gas environments, facilitating detailed kinetic studies of materials during laser heating.

Contribution

The development of a novel laser reaction chamber that supports dynamic heating and operando XRD measurements under vacuum and gas conditions at NSLS-II.

Findings

Resolved chemical reaction kinetics with 1-s time resolution.

Demonstrated capabilities with iron oxide and WTe2 samples.

Enabled in-situ studies of bulk and single crystal materials.

Abstract

We present a laser reaction chamber that we developed for in-situ/operando X-ray diffraction measurements at the NSLS-II 28-ID-2 XPD (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 XRD studies in both bulk and single crystal materials.