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Abstract: Continuous technological advancement and depleting natural sources of key metals such as gold necessitate highly selective recovery processes from secondary sources. Herein, we report the visualisation of a recyclable precipitation process using dual imaging and diffraction that gives insight into the mechanism of precipitation and highlights the possibility of kinetic separations.

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Abstract: Thick electrodes are a promising route to increase battery energy density by increasing the fraction of active material relative to inactive components. However, at high cycling rates, greater mass transport limitations in thick electrodes can lead to poor capacity utilisation and reduced power density. Although advanced electrode structuring strategies have been explored, many require expensive manufacturing changes or complex post-processing. An alternative approach uses standard battery manufacturing methods to sequentially coat active materials with different particle sizes or compositions. In this work, polycrystalline LiNi1/3Mn1/3Co1/3O2 (NMC111) particles of two sizes were used to fabricate particle size-graded bilayer electrodes. An impedance-based finite element model was developed to evaluate transport properties in the graded structures and was validated using electrochemical impedance spectroscopy (EIS) and rate tests. Operando synchrotron diffraction revealed a more homogeneous state of charge when smaller particles were positioned near the separator and larger particles near the current collector. Together, the modelling and experimental results show that simple particle size grading improves ion transport and reaction uniformity, enhancing capacity utilisation. This approach offers a practical pathway to improve the power performance of next-generation battery electrodes.

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Abstract: Utilizing green and renewable materials derived from biological sources is crucial for reducing environmental pollution. Natural wood is a clean and sustainable material. Densification methods have been shown to greatly enhance the mechanical properties of wood. However, the inherent hydrophilic and hygroexpansion characteristics of wood significantly limit the application of densified wood in various engineering fields. This study aimed to investigate the water absorption behavior and dimensional stability of natural and densified pine through water absorption experiments. The results showed that densified pine exhibited a similar three-stage water absorption behavior to that of natural pine. The water absorption behavior of densified pine caused by diffusion of water molecules as bound water in the cell wall (stage I), conforming to the Fickian model. In the subsequent stage II, excess water in the cell wall diffused into the cell lumen as free water. The water absorption behavior then deviated from the Fickian model and followed the Langmuir model. The significant reduction in the equilibrium moisture content of densified pine, compared to natural pine, can be attributed to a decrease in hemicellulose as well as smaller cell interstices and lumens. Moreover, unlike natural pine, where hygroexpansion was only in stage Ⅰ, densified pine expanded further in stage Ⅱ due to partial recovery of the cell lumen. Nuclear magnetic resonance (NMR), Fourier-transform infrared (FT-IR), Scanning electron microscopy (SEM) and X-ray computed tomography and diffraction techniques were employed to elucidate the effect of densification on dimensional stability and water absorption behavior of pine.

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Abstract: Anode-free solid-state batteries (AF-SSBs) hold great promise for next-generation transportation electrification, offering improved safety, recyclability, and high performance (energy density >1500 Wh/L, specific energy >500 Wh/kg) at reduced cost (<$100/kWh) compared to conventional Li-ion batteries. However, their practical deployment is hindered by poor chemo-mechanical stability at the evolving anode|solid electrolyte (SE) interface, where localized ionic flux during cycling drives dendrite formation, internal short-circuiting, and premature failure. The buried and dynamic nature of this interface makes direct characterization especially challenging, and existing methods lack the ability to capture non-invasive, 3D operando insights into interfacial morphology, spatial dynamics, and strain evolution in full-cell AF-SSBs. In this work, we conducted operando correlative synchrotron X-ray micro-computed tomography (XCT) and X-ray diffraction (XRD) at the DIAD beamline, Diamond Light Source (UK), to map interface evolution in real time. Custom PEEK-housed tube cells were cycled at 35 µA (2 mm Li | 19 mg LPSC | 3 mm stainless steel), with 13 tomographic scans collected across three charge–discharge cycles prior to short-circuiting. XCT resolved void formation, crack initiation, and fracture propagation, while XRD provided spatially resolved strain mapping and crystallographic fingerprints of interfacial contact evolution. Our imaging data revealed pre-existing cracks within the SE pellet, as well as the nucleation of new spallation-like cracks originating at the current collector–SE interface that widened progressively during cycling. XRD mapping confirmed that these cracks coincided with regions of strain accumulation and interfacial delamination, offering a crystallographic fingerprint of contact evolution. Importantly, these structural changes could be directly correlated with electrochemical signatures: the onset of fracture formation aligned with abrupt cell polarization and preceded catastrophic short-circuiting. Together, this correlative XCT–XRD methodology provides the integrated view of how morphology, strain, and electrochemistry couple to govern failure in AF-SSBs.

Open Access

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Abstract: Understanding the interactions between microstructure, strain, phase and material behavior is crucial in scientific fields such as energy storage, carbon sequestration and biomedical engineering. However, quantifying these correlations is challenging, as it requires the use of multiple instruments and techniques, often separated by space and time. The Dual Imaging and Diffraction (DIAD) beamline at Diamond Light Source is designed to address this challenge. DIAD allows its users to visualize internal structures (in two and three dimensions), identify compositional/phase changes and measure strain. It enables in situ and operando experiments that require spatially correlated information. DIAD provides two independent beams combined at one sample position, allowing `quasi-simultaneous' X-ray computed tomography and X-ray powder diffraction. A unique functionality of the DIAD configuration is the ability to perform `image-guided diffraction', where the micrometre-sized diffraction beam is scanned over the complete area of the imaging field of view without moving the specimen. This moving-beam diffraction geometry enables the study of fast-evolving and motion-susceptible processes and samples. Here, we discuss the novel moving-beam diffraction geometry, presenting the latest findings on the reliability of both the geometry calibration and the data-reduction routines used. We provide a comprehensive quantitative assessment of the moving-beam diffraction geometry implemented at the DIAD beamline, which will serve as a reference for beamline users. Our measurements confirm that diffraction is most sensitive to the moving-beam geometry for the conventional transmission geometry of the detector. The observed data confirm that the motion of the Kirkpatrick–Baez mirror coupled with a fixed-aperture slit results in a rigid translation of the beam probe, without affecting the angle of the incident-beam path to the sample. Our measurements demonstrate that a nearest-neighbor calibration can achieve the same accuracy as a self-calibrated geometry when the distance between the calibrated and probed sample regions is smaller than or equal to the beam spot size. The absolute error of the moving-beam diffraction geometry at DIAD with typical calibration setup remains below 0.01%, which is the accuracy we observe for the beamline with stable beam operation.