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Communications Physics 3(1), 97 (2020). doi:10.1038/s42005-020-0362-y, The emergence of high repetition-rate X-ray free-electron lasers (XFELs) powered by superconducting accelerator technology enables the measurement of significantly more experimental data per day than was previously possible. The European XFEL is expected to provide 27,000 pulses per second, over two orders of magnitude more than any other XFEL. The increased pulse rate is a key enabling factor for single-particle X-ray diffractive imaging, which relies on averaging the weak diffraction signal from single biological particles. Taking full advantage of this new capability requires that all experimental steps, from sample preparation and delivery to the acquisition of diffraction patterns, are compatible with the increased pulse repetition rate. Here, we show that single-particle imaging can be performed using X-ray pulses at megahertz repetition rates. The results obtained pave the way towards exploiting high repetition-rate X-ray free-electron lasers for single-particle imaging at their full repetition rate., Published by Springer Nature, London

Optica 6(9), 1106 - 1109 (2019). doi:10.1364/OPTICA.6.001106, Modern emerging technologies, such as additive manufacturing, bioprinting, and new material production, require novel metrology tools to probe fundamental high-speed dynamics happening in such systems. Here we demonstrate the application of the megahertz (MHz) European X-ray Free-Electron Laser (EuXFEL) to image the fast stochastic processes induced by a laser on water-filled capillaries with micrometer-scale spatial resolution. The EuXFEL provides superior contrast and spatial resolution compared to equivalent state-of-the-art synchrotron experiments. This work opens up new possibilities for the characterization of MHz stochastic processes on the nanosecond to microsecond time scales with object velocities up to a few kilometers per second using XFEL sources., Published by OSA, Washington, DC

Interactions between neighboring grains influence the macroscale behavior of polycrystalline materials, particularly their deformation behavior, damage initiation and propagation mechanisms. However, mapping all of the critical material properties normally requires that several independent measurements are performed. Here we report the first grain mapping of a polycrystalline foil using a pixelated energy-dispersive X-ray area detector, simultaneously measuring X-ray fluorescence and diffraction with the Maia detector in order to determine grain orientation and estimate lattice strain. These results demonstrate the potential of the next generation of X-ray area detectors for materials characterization. By scanning the incident X-ray energy we investigate these detectors as a complete solution for simultaneously mapping the crystallographic and chemical properties of the sample. The extension of these techniques to broadband X-ray sources is also discussed.

Elemental, chemical, and structural analysis of polycrystalline materials at the micron scale is frequently carried out using microfocused synchrotron X-ray beams, sometimes on multiple instruments. The Maia pixelated energy-dispersive X-ray area detector enables the simultaneous collection of X-ray fluorescence (XRF) and diffraction because of the relatively large solid angle and number of pixels when compared with other systems. The large solid angle also permits extraction of surface topography because of changes in self-absorption. This work demonstrates the capability of the Maia detector for simultaneous measurement of XRF and diffraction for mapping the short- and long-range order across the grain structure in a Ni polycrystalline foil.

Optica 7(6), 716 - (2020). doi:10.1364/OPTICA.396728, A critical challenge of pump-probe experiments with x-ray free-electron lasers (XFELs) is accurate synchronization of x-ray and optical pulses. At the European XFEL we observed megahertz rate timing jitter of 24.0±12.4fs., Published by OSA, Washington, DC

We report on the development and implementation of single-shot hard X-ray/optical cross-correlation at the European X-ray free-electron laser for characterization of timing jitter and drift at megahertz rate.

Energy-resolved neutron imaging experiments conducted on the Small Angle Neutron Scattering (SANS) instrument, Bilby, demonstrate how the capabilities of this instrument can be enhanced by a relatively simple addition of a compact neutron counting detector. Together with possible SANS sample surveying and location of the region of interest, this instrument is attractive for many imaging applications. In particular, the combination of the cold spectrum of the neutron beam and its pulsed nature enables unique non-destructive studies of the internal structure for samples that are opaque to other more traditional techniques. In addition to conventional white beam neutron radiography, we conducted energy-resolved imaging experiments capable of resolving features related to microstructure in crystalline materials with a spatial resolution down to ∼0.1 mm. The optimized settings for the beamline configuration were determined for the imaging modality, where the compromise between the beam intensity and the achievable spatial resolution is of key concern.

Optics letters 44(7), 1650 - 1653 (2019). doi:10.1364/OL.44.001650, Intense, ultrashort, and high-repetition-rate X-ray pulses, combined with a femtosecond optical laser, allow pump-probe experiments with fast data acquisition and femtosecond time resolution. However, the relative timing of the X-ray pulses and the optical laser pulses can be controlled only to a level of the intrinsic error of the instrument which, without characterization, limits the time resolution of experiments. This limitation inevitably calls for a precise determination of the relative arrival time, which can be used after measurement for sorting and tagging the experimental data to a much finer resolution than it can be controlled to. The observed root-mean-square timing jitter between the X-ray and the optical laser at the SPB/SFX instrument at European XFEL was 308 fs. This first measurement of timing jitter at the European XFEL provides an important step in realizing ultrafast experiments at this novel X-ray source. A method for determining the change in the complex refractive index of samples is also presented., Published by OSA, Washington, DC

Determining bulk residual elastic strains is a topic of critical importance for predictive modelling and materials testing. Although there are numerous approaches to obtaining this information the process is often time-consuming and frequentlyinvolves destructive sectioning of the sample. This paper presents the latest developments in Bragg-edge neutron strain tomography which offers a rapid, non-destructive means of determining residual elastic strains in polycrystalline materials with high spatial resolution.Neutron strain tomography utilises the fact that the energy-resolved transmission spectrum of thermal neutrons froma polycrystalline sample displays well-defined, sudden jumps in intensity known as ‘Bragg-edges’, which reveal information about the average residual elastic strain throughout the sample volume. By measuring the spatially resolved transmission spectrum for a number of different sample orientations it is possible to recover the underlying three-dimensional residual elastic strain profile. This process is analogous to conventional absorption tomography where a three-dimensional map of the sample density is recovered from a lower order two-dimensional set of integral absorption measurements. Using the newly developed microchannel plate TimePix neutron detectorin time-of-flight experiments, elastic strains can in principle be recovered with 10 um spatial resolution. The current work demonstrates a model-free method for direct inversion of the average strain profiles obtained from Bragg-edge measurements using results from linear elasticity theory and the Radon transform, which is the basis for absorption tomography reconstructions. We demonstrate this method in simulation on an axisymmetric sample with analytic strain profile before applying it to a ‘real-world’ sample where the results are validated against conventional neutron diffraction and hole drilling measurements.

Journal of synchrotron radiation 24(1), 83 - 94(2017). doi:10.1107/S1600577516017525, The proliferation of extremely intense synchrotron sources has enabled ever higher-resolution structures to be obtained using data collected from smaller and often more imperfect biological crystals (Helliwell, 1984). Synchrotron beamlines now exist that are capable of measuring data from single crystals that are just a few micrometres in size. This provides renewed motivation to study and understand the radiation damage behaviour of small protein crystals. Reciprocal-space mapping and Bragg coherent diffractive imaging experiments have been performed on cryo-cooled microcrystals of hen egg-white lysozyme as they undergo radiation damage. Several well established metrics, such as intensity-loss and lattice expansion, are applied to the diffraction data and the results are compared with several new metrics that can be extracted from the coherent imaging experiments. Individually some of these metrics are inconclusive. However, combining metrics, the results suggest that radiation damage behaviour in protein micro-crystals differs from that of larger protein crystals and may allow them to continue to diffract for longer. A possible mechanism to account for these observations is proposed., Published by IUCr, Chester

Using recently developed microchannel plate (MCP) neutron area detectors at a pulsed neutron source provides a method of fast non-destructive imaging and characterisation of advanced materials at unprecedented spatial resolution. The energy resolved neutron transmission spectrum can be found from the neutron time of flight (ToF), this provides valuable information about the crystallographic structure within the sample such as the average residual elastic strain in the incident beam direction. By measuring this spectrum at a number of sample orientations information is built up about the strain distribution throughout the specimen. The energy-resolved neutron transmission spectrum of an additively manufactured turbine blade was measured at the Engin-X instrument, ISIS, UK. A high resolution three-dimensional reconstruction of the neutron attenuation coefficient of the blade was recovered, then analysis of the energy resolved spectrum gave insight into the underlying residual elastic strain profile imparted by the advanced manufacturing process.

Three-dimensional imaging of protein crystals during x-ray diffraction experiments opens up a range of possibilities for optimizing crystal quality and gaining new insights into the fundamental processes that drive radiation damage. Obtaining this information at the appropriate length-scales however is extremely challenging. One approach that has been recently demonstrated as a promising avenue for characterizing the size and shape of protein crystals at nanometre length-scales is Bragg coherent diffractive imaging (BCDI). BCDI is a recently developed technique that is able to recover the phase of the continuous diffraction intensity signal around individual Bragg peaks. When data is collected at multiple points on a rocking curve, a reciprocal space map (RSM) can be assembled and then inverted using BCDI to obtain a three-dimensional image of the crystal. The first demonstration of two-dimensional biological BCDI was reported by Boutet et al on holoferritin, recently this work was extended to the study of radiation damage in micron-sized protein crystals. Here we present the first three-dimensional reconstructions of a Lysozyme protein crystal using BDI. The results are validated against RSM and transmission electron microscopy data and have implications for both radiation damage studies and for developing new approaches for structure retrieval from micron-sized protein crystals.