A high-temperature sample changer for parallelized in situ X-ray studies to efficiently explore reaction space

Abstract

A sample environment for high-throughput X-ray scattering studies in transmission geometry to probe the mechanism and kinetics of moderate-temperature reactions in solution, molten fluxes and solids is described. This high-temperature sample changer enables efficient studies of reactions that are slow relative to the timescale of the X-ray scattering measurements by allowing up to 18 samples to be probed at the same temperature in parallel. This significantly enhances the throughput of in situ X-ray scattering studies as the sample changer effectively facilitates systematic studies that compare different reaction parameters (e.g. concentration, precursor, composition, additives), reference samples (e.g. background, pure precursors) and replicates (to demonstrate reproducibility) with enhanced consistency afforded by the quasi-simultaneous nature of the measurements. The large sample volumes, compared with those typically used for X-ray scattering measurements, are on a similar scale to those in the laboratory, making the results more directly comparable.