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Abstract: X-ray computed tomography (XCT) is regularly employed in geomechanics to non-destructively measure the solid and pore fractions of soil and rock from reconstructed 3D images. With the increasing availability of high-resolution XCT imaging systems, researchers now seek to measure microfabric parameters such as the number and area of interparticle contacts, which can then be used to inform soil behaviour modelling techniques. However, recent research has evidenced that conventional image processing methods consistently overestimate the number and area of interparticle contacts, mainly due to acquisition-driven image artefacts. The present study seeks to address this issue by systematically assessing the role of XCT acquisition parameters in the accurate detection of interparticle contacts. To this end, synchrotron XCT has been applied to a hexagonal close-packed arrangement of glass pellets with and without a prescribed separation between lattice layers. Different values for the number of projections, exposure time, and rotation range have been evaluated. Conventional global grey value thresholding and novel U-Net segmentation methods have been assessed, followed by local refinements at the presumptive contacts, as per recently proposed contact detection routines. The effect of the different acquisition set-ups and segmentation techniques on contact detection performance is presented and discussed, and optimised workflows are proposed.

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Abstract: Zero carbon energy generation from renewable sources can reduce climate change by mitigating carbon emissions. A major challenge of renewable energy generation is the imbalance between supply and demand. To overcome the energy imbalances, subsurface storage of hydrogen in porous mediais suggested as a large-scale and economic solution, yet its mechanisms are not fully understood. Important unknowns are the effect of the high migration potential of the small and mobile hydrogen molecule and the volume of recoverable hydrogen. We conducted non-steady state, cyclic hydrogen and brine injection experiments at 2-7 MPa and flow rates of 2-80 µl min-1 using water-wet Clashach sandstone cylinders of 4.7 mm diameter and 53-57 mm length (Clashach composition: ~96 wt.% quartz, 2% K-feldspar, 1% calcite, 1% ankerite). Two sets of experiments were performed using our new transparent flow-cell designed for x-ray computed microtomography: 1) Experiments using a laboratory x-ray source (University of Edinburgh) imaged the flow, displacement and capillary trapping of hydrogen by brine as a function of saturation after primary drainage and secondary imbibition. 2) Experiments using synchrotron radiation (Diamond Light Source, I12-JEEP tomography beamline) captured time-resolved hydrogen and brine flow and displacement processes. Pressure and mass flow measurements across the experimental apparatus complemented the microtomography volumes in both sets of experiments. Results from a water-wet rock show that hydrogen behaves as a non-wetting phase and sits in the centre of the pore bodies, while residual brine sits in corners and pore throats. Hydrogen saturation in the pore volume is independent of the injection pressure and increases with increasing hydrogen/brine injection ratio up to ~50% saturation at 100 % hydrogen. Capillary trapping of hydrogen during brine imbibition occurs via snap off and is greatest at higher brine injection pressures, with 10 %, 12% and 21% hydrogen trapped at 2, 5 and 7 MPa, respectively. Higher brine flow rates reduce capillary trapping and increase hydrogen recovery at any given injection pressure. Based on these results, future hydrogen storage operations should inject 100% hydrogen and manage the reservoir pressure to avoid high pressures and minimize capillary trapping of hydrogen during brine reinjection. Ongoing analysis of time-resolved experimental data will provide further insight into the critical pore-scale processes that ultimately influence the potential for geological hydrogen storage and recovery.

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Abstract: Ductile cast irons (DCIs) are of increasing importance in the renewable energy and transportation sectors. The distribution and morphology of the graphite nodules, in particular the formation of degenerate features during solidification, dictate the mechanical performance of DCIs. In situ high-speed synchrotron X-ray tomography was used to capture the evolution of graphite nodules during solidification of DCI, including degenerate features and the effect of the carbon concentration field. The degeneration of nodules is observed to increase with re-melting cycles, which is attributed to Mg-loss. The dendritic primary austenite and carbon concentration gradients in the surrounding liquid phase were found to control nodule morphology by locally restricting and promoting growth. A coupled diffusion-mechanical model was developed, confirming the experimentally informed hypothesis that protrusions form through liquation cracking of the austenite shell and subsequent localised growth. These results provide valuable insights into the solidification kinetics of cast irons, supporting the design of advanced alloys.

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Abstract: Crystallisation is a complex process that significantly affects the rheology of magma, and thus the flow dynamics during a volcanic eruption. For example, the evolution of crystal fraction, size and shape has a strong impact on the surface crust formation of a lava flow, and accessing such information is essential for accurate modelling of lava flow dynamics. To investigate the role of crystallisation kinetics on lava flow behaviour, we performed real-time, in situ synchrotron X-ray microtomography, studying the influence of temperature-time paths on the nucleation and growth of clinopyroxene and plagioclase in an oxidised, nominally anhydrous basaltic magma. Crystallisation experiments were performed at atmospheric pressure in air and temperatures from 1250 °C to 1100 °C, using a bespoke high-temperature resistance furnace. Depending on the cooling regime (single step versus continuous), two different crystal phases (either clinopyroxene or plagioclase) were produced, and we quantified their growth from both global and individual 3D texture analyses. The textural evolution of charges suggests that suppression of crystal nucleation is due to changes in the melt composition with increasing undercooling and time. Using existing viscosity models, we inferred the effect of crystals on the viscosity evolution of our crystal-bearing samples to trace changes in rheological behaviour during lava emplacement. We observe that under continuous cooling, both the onsets of the pāhoehoe-‘a‘ā transition and of non-Newtonian behaviour occur within a shorter time frame. With varying both temperature and time, we also either reproduced or approached the clinopyroxene and plagioclase phenocryst abundances and compositions of the Etna lava used as starting material, demonstrating that real-time synchrotron X-ray tomography is an ideal approach to unravel the final solidification history of basaltic lavas. This imaging technology has indeed the potential to provide input into lava flow models and hence our ability to forecast volcanic hazards.

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Abstract: The governing mechanistic behaviour of Directed Energy Deposition Additive Manufacturing (DED-AM) is revealed by a combined in situ and operando synchrotron X-ray imaging and diffraction study of a nickel-base superalloy, IN718. Using a unique DAE-AM process replicator, real-space imaging enables quantification of the melt-pool boundary and flow dynamics during solidification. This imaging knowledge was also used to informed precise diffraction measurements of temporally resolved microstructural phases during transformation and stress development with a spatial resolution of 100 µm. The diffraction quantified thermal gradient enabled a dendritic solidification microstructure to be predicted and coupled to the stress orientation and magnitude. The fast cooling rate entirely suppressed the formation of secondary phases or recrystallisation in the solid-state. Upon solidification, the stresses rapidly increase to the yield strength during cooling. This insight, combined with the large solidification range of IN718 suggests that the accumulated plasticity exhausts the ductility of the alloy, causing liquation cracking. This study has revealed additional fundamental mechanisms governing the formation of highly non-equilibrium microstructures during DED-AM.