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S C I E N T I F I C H I G H L I G H T S

S T R U C T U R E O F M A T E R I A L S

The Structure of Materials group provides facilities for a range of X-ray scattering, imaging and spectroscopy experiments, relevant to the fields of energy research, catalysis, engineering, metallurgy, nanoscience and other fields of advanced technology. In addition to these traditional technological subjects, the Structure of Materials group also covers X-ray imaging studies for biology, archaeology and palaeontology.

In 2022, beamline BM05 continued to offer a significant amount of beamtime for various commercial experiments using the tomography and topography end-stations, as well as for commercial instrumentation development. From 2023 onwards, the beamline will also be open for standard proposals to exploit the propagation phase- contrast tomography station, covering pixel sizes from 25 µm to 0.3 µm. The beamline also houses a new sample environment table, facilitating the installation of equipment such as an induction furnace or a cryostream for in-situ experiments.

The dark-field X-ray microscopy (DFXM) project was selected as EBS beamline EBSL2 and is currently being implemented on ID03. DFXM is a non-destructive technique that can provide 3D maps of lattice strain and orientation, offering unique insights into the crystal structure of materials on length scales from 100 μm to 100 nm. Samples come from a wide range of scientific fields including structural materials such as metals and alloys, functional materials such as ferroelectrics, and semiconductors and biominerals. The existing experimental station is being dismantled from ID06-HXM and will be transferred to the new dark-field microscopy beamline ID03. Consequently, ID06-HXM concluded its short user programme in October 2022. We expect to start commissioning EBSL2 in September 2023, with the goal to resume user operations in March 2024, i.e., accepting general user proposals for the September 2023 deadline. As a full beamline dedicated to DFXM, it will effectively double the amount of beamtime available to the user

community. Finally, we have made significant progress in the development of the data analysis package, DARFIX, which provides a set of computer vision techniques for the analysis of DFXM data.

2022 was a busy year of operation at the Materials Science beamline ID11. All of the user experiments that were delayed due to the pandemic were completed, and the backlog has now been cleared. New aluminium compound reflective lenses have recently been installed for the nanoscope end-station, and these offer higher fluxes for larger beam sizes (around 1 μm) as a complementary option to the nanofocusing optics for larger fields of view. Work is in progress to allow the Eiger 4M CdTe detector to be used safely on the 3D X-ray diffraction (XRD) station in addition to the nanofocus station, and we hope this will be completed in 2023. The beamline continues to offer a wide range of high-energy X-ray diffraction methods for imaging atomic structures in materials. Scanning methods using small X-ray beams are benefitting strongly from the high frame rates available with the Eiger detector. The suite of methods using imaging detectors (DCT, topotomography) are now well integrated into the new Bliss control system thanks to developments delivered within the framework of a long-term proposal.

The main areas of activity of ID15A are battery science, catalysis and the study of glasses and other disordered systems. ID15A is optimised for the rapid acquisition (up to 500 Hz) of multi-dimensional, multi-resolution X-ray diffraction data on real devices. New data acquisition strategies for XRD-CT have recently been developed to allow mapping with high spatial resolution of selected small regions inside large objects. Software tools for real time XRD-CT data processing, based on parallel processing, are now available for the user community. In 2022, the beamline team, in collaboration with the ID27 team, performed the first XRD experiments with a multi- channel collimator at very high energy (100 keV). It is now possible, for the first time, to study the interior of large heterogeneous samples, such as large battery formats,