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High-throughput powder diffraction on beamline I11 at Diamond

DOI: 10.1107/S0021889810044948 DOI Help

Authors: Julia Parker (Diamond Light Source) , Stephen Thompson (Diamond Light Source) , Tom Cobb (Diamond Light Source) , Fajin Yuan (Diamond Light Source) , Jonathan Potter (Diamond Light Source) , Alistair Lennie (Diamond Light Source) , Sam Alexander (Johnson Matthey) , Christopher Tighe (UCL Chemistry) , Jawwad Darr (University College London) , Jeremy Cockcroft (University College London) , Chiu Tang (Diamond Light Source)
Co-authored by industrial partner: No

Type: Journal Paper
Journal: Journal Of Applied Crystallography , VOL 44 (1) , PAGES 102-110

State: Published (Approved)
Published: February 2011

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, TiO2 and TiO2/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 La4Ni3-xFexO10 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.

Journal Keywords: Powder Diffraction; Synchrotron Radiation; High-Throughput Structural Analysis

Subject Areas: Technique Development

Instruments: I11-High Resolution Powder Diffraction