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Abstract: High-speed synchrotron tomography was used to investigate the nucleation and growth dynamics of Al13Fe4 intermetallic during solidification of an Al-5wt%Fe alloy, providing new insights into its formation process. The majority of Al13Fe4 intermetallics nucleated near the surface oxide of the specimen and a few nucleated at Al13Fe4 phase. Al13Fe4 crystals grew into a variety of shapes, including plate-like, hexagonal tabular, stair-like and V-shaped, which can be attributed to the crystal structure of this compound and its susceptibility to twinning. Hole-like defects filled with aluminium melt were observed within the intermetallics. Oriented particle attachment mechanism was proposed to explain the formation of the Al13Fe4 intermetallic, which needs further experiments and simulation to confirm.

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Abstract: An experimental technique is described for the collection of time-resolved X-ray diffraction information from a complete commercial battery cell during discharging or charging cycles. The technique uses an 80 × 80 pixel 2D energy-discriminating detector in a pinhole camera geometry which can be used with a polychromatic X-ray source. The concept was proved in a synchrotron X-ray study of commercial alkaline Zn–MnO2 AA size cells. Importantly, no modification of the cell was required. The technique enabled spatial and temporal changes to be observed with a time resolution of 20 min (5 min of data collection with a 15 min wait between scans). Chemical changes in the cell determined from diffraction information were correlated with complementary X-ray tomography scans performed on similar cells from the same batch. The clearest results were for the spatial and temporal changes in the Zn anode. Spatially, there was a sequential transformation of Zn to ZnO in the direction from the separator towards the current collector. Temporally, it was possible to track the transformation of Zn to ZnO during the discharge and follow the corresponding changes in the cathode.

Open Access

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Abstract: The Directed Energy Deposition Additive Manufacturing (DED-AM) of SS316L was studied using in situ and operando synchrotron X-ray imaging to quantitively understand the effect of processing parameters on the melt-pool morphology and surface quality. It was found that surface roughness of DED-AM builds can result from melt pool surface perturbations caused by changes in the melt flow and build stage motion perturbations. Process maps are developed that quantitatively correlate build quality to process parameters including powder feed rate, laser power and traverse speed. How the AM process parameters control build efficacy is clarified, and the processing conditions required to dampen surface perturbations leading to roughness were determined.

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Abstract: A key technique for controlling solidification microstructures is magneto-hydrodynamics (MHD), resulting from imposing a magnetic field to solidifying metals and alloys. Applications range from bulk stirring to flow control and turbulence damping via the induced Lorentz force. Over the past two decades the Lorentz force caused by the interaction of thermoelectric currents and the magnetic field, a MHD phenomenon known as Thermoelectric Magnetohydrodynamics (TEMHD), was also shown to drive inter-dendritic flow altering microstructural evolution. In this contribution, high-speed synchrotron X-ray tomography and computational simulation are coupled to reveal the evolution, dynamics and mechanisms of solidification within a magnetic field, resolving the complex interplay and competing flow effects arising from Lorentz forces of different origins. The study enabled us to reveal the mechanisms disrupting the traditional columnar dendritic solidification microstructure, ranging from an Archimedes screw-like structure, to one with a highly refined dendritic primary array. We also demonstrate that alloy composition can be tailored to increase or decrease the influence of MHD depending on the Seebeck coefficient and relative density of the primary phase and interdendritic liquid. This work paves the way towards novel computational and experimental methods of exploiting and optimising the application of MHD in solidification processes, together with the calculated design of novel alloys that utilise these forces.

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Abstract: Soil organic carbon (SOC) is of key importance for soil functioning. It strongly impacts soil fertility, greenhouse gas emissions, nutrient retention, and contaminant degradation. The soil pore network determines how oxygen, water and nutrients are transported and exchanged in soil, and the architecture of the soil is therefore equally fundamental to soil functions. For a thorough understanding of the microbial habitat, the soil pore network architecture needs to be evaluated alongside with the spatial distribution of SOC, but the challenge ahead is the 3-D visualization of organic carbon at the micro-scale. At present, such visualizations are undertaken using staining agents, but their non-specific binding to other features in the soil aggravates evaluation of organic carbon at the micro-scale. In the present study, we investigated the potential and limitations of using joint white-beam neutron and X-ray imaging for mapping the 3-dimensional organic carbon distribution in soil. This approach is viable because neutron and X-ray beams have complementary attenuation properties. Soil minerals consist to a large part of silicon and aluminium, elements which are relatively translucent to neutrons but attenuate X-rays. In contrast, attenuation of neutrons is strong for hydrogen, which is abundant in SOC, while hydrogen barely attenuates X-rays. When considering dried soil samples, the complementary attenuation for neutrons and X-rays may be used to quantify the fractions of air, SOC and minerals for any imaged voxel in a bi-modal 3-dimensional image, i.e. a combined neutron and X-ray image. We collected neutron data at the IMAT beamline at the ISIS facility and X-ray data at the I12 beamline at the Diamond Light source, both located within the Rutherford Appleton Laboratory, Harwell, UK. The neutron image clearly showed variations in neutron attenuation within soil aggregates at approximately constant X-ray attenuations. This indicates a constant bulk density with varying organic matter and/or mineralogy. For samples with identical mineral composition, neutron attenuation data of sieved and repacked soil samples exhibited a large coefficient of determination (R2) in a regression between volumetric SOC content and neutron attenuation (0.9). Even larger R2 (0.93) were obtained when the volumetric clay content was also included into the regression. However, when comparing soil samples with different mineralogy, R2 dropped to 0.24 and 0.37, depending whether the clay content was considered or not. To improve the method, it is necessary to include specifics of the soil mineralogy. Here, analysing the time-of-flight neutron attenuation data collected at the IMAT beamline will provide further insights. In summary, our approach yielded promising results. We anticipate that quantitative 3-D imaging of organic carbon contents in soil will be possible in the near future.