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, 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.

Photoluminescence of cerium-doped (Ca1−xSrx)3RE2Ge3O12 garnet phosphors for solid state lighting: Relating structure to emission

“…Laboratory powder X-ray diffraction (PXRD) data were obtained on a Bruker D8 diffractometer (Bragg-Brentano geometry) using Cu-K a radiation and a position sensitive detector (LynxEye). Synchrotron PXRD data were collected at the Diamond Light Source, Harwell Research Laboratories, Oxfordshire, UK, on beamline I11 (k = 0.826 Å) using a multianalysing crystal detector array [20,21]. The Rietveld method was used to refine structural parameters using the program FULLPROF [22].…”

Parameterization of the coupling between strain and order parameter for LuF[SeO3]

“…Powder diffraction data from LuF[SeO 3 ] were collected at the high-resolution powder diffractometer I11 at Diamond, UK (Parker et al, 2011;Thompson et al, 2009Thompson et al, , 2011. The wavelength was determined to be 0.8264 (3) Å from a silicon standard.…”

Jahn-Teller induced nematic orbital order in tetragonalSr2VO4

“…given in appendix, details of the beamiline are reported in [15,16]). The samples were prepared by reduction of Sr 4 V 2 O 9 in a sealed quartz tube with zirconium as an oxygen getter [17].…”

“…Structural studies were performed through X-ray diffraction experiments on powder samples. Measurements were done at synchrotron facility at Diamond Light Source, by using the I11 beamline [15]. The Xray beam was monochromatized at E = 15 keV (λ = 0.82713Å).…”