High-throughput powder diffraction on beamline I11 at Diamond

Abstract

A new capability designed for high-throughput (HT) structural analysis using the synchrotron powder diffraction beamline (I11) at Diamond Light Source is reported. With a high-brightness X-ray beam, multi-analyser detectors and fast data-acquisition procedures, high-quality diffraction data can be collected at a speed of ∼15–30 min per powder pattern for good crystalline materials. Fast sample changing at a rate of a few seconds per specimen is achieved with a robotic arm and pre-loaded capillary specimens on a multi-tray carousel (200-sample capacity). Additional equipment, such as an automatic powder-loading machine and a pre-alignment jig for the sample capillaries, is available to reduce preparation time. For demonstration purposes, the first results presented here are those from standard reference powders of Si, TiO 2 and TiO 2 /Si mixtures, obtained by analysing the data using Le Bail (instrumental calibration) and Rietveld refinements (quantitative agreement within 1%). The HT hardware was then used to study the structural phase evolution of a library of 31 La 4 Ni 3− x Fe x O 10 heterometallic ceramic powders in less than 1 d. The powders were generated from a single heat treatment (at 1348 K in air for 12 h) of nanoceramic oxide co-precipitate precursors, made using a newly developed HT synthesis robot. Crystallographic details (symmetry and lattice parameters) were obtained as a function of Fe concentration. The results revealed that this approach was able to produce a pure Ruddlesden–Popper-type phase with an iron content of up to x = 0.5, significantly higher than has been achieved previously using more conventional synthesis routes and thus demonstrating the power of using the HT approach.