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  1. Free, publicly-accessible full text available September 1, 2023
  2. Electrification of the transportation sector relies on radical re-imagining of energy storage technologies to provide affordable, high energy density, durable and safe systems. Next generation energy storage systems will need to leverage high energy density anodes and high voltage cathodes to achieve the required performance metrics (longer vehicle range, long life, production costs, safety). Solid-state batteries (SSBs) are promising materials technology for achieving these metrics by enabling these electrode systems due to the underlying material properties of the solid electrolyte ( viz. mechanical strength, electrochemical stability, ionic conductivity). Electro-chemo-mechanical degradation in SSBs detrimentally impact the Coulombic efficiencies, capacity retention, durability and safety in SSBs restricting their practical implementation. Solid|solid interfaces in SSBs are hot-spots of dynamics that contribute to the degradation of SSBs. Characterizing and understanding the processes at the solid|solid interfaces in SSBs is crucial towards designing of resilient, durable, high energy density SSBs. This work provides a comprehensive and critical summary of the SSB characterization with a focus on in situ and operando studies. Additionally, perspectives on experimental design, emerging characterization techniques and data analysis methods are provided. This work provides a thorough analysis of current status of SSB characterization as well as highlights important avenues for futuremore »work.« less
  3. Rock salt caverns have been extensively used as reliable repositories for hazardous waste such as nuclear waste, oil or compressed gases. Undisturbed rock salt deposits in nature are usually impermeable and have very low porosity. However, rock salt formations under excavation stresses can develop crack networks, which increase their porosities; and in the case of a connected crack network within the media, rock salt may become permeable. Although the relationship between the permeability of rock salt and the applied stresses has been reported in the literature, a microscopic study that investigates the properties influencing this relationship, such as the evolution of texture and internal stresses, has yet to be conducted. This study employs in situ 3D synchrotron micro-computed tomography and 3D X-ray diffraction (3DXRD) on two small-scale polycrystalline rock salt specimens to investigate the evolution of the texture and internal stresses within the specimens. The 3DXRD technique measures the 3D crystal structure and lattice strains within rock salt grains. The specimens were prepared under 1D compression conditions and have shown an initial {111} preferred texture, a dominant {110}〈1 1 0〉 slip system and no fully connected crack network. The {111} preferred texture under the unconfined compression experiment became stronger, whilemore »the {111}〈1 1 0〉 slip system became more prominent. The specimens did not have a fully connected crack network until applied axial stresses reached about 30 MPa, at a point where the impermeability of the material becomes compromised due to the development of multiple major cracks.« less
  4. Abstract

    The solidification mechanism and segregation behavior of laser-melted Mn35Fe5Co20Ni20Cu20was firstly investigated via in situ synchrotron x-ray diffraction at millisecond temporal resolution. The transient composition evolution of the random solid solution during sequential solidification of dendritic and interdendritic regions complicates the analysis of synchrotron diffraction data via any single conventional tool, such as Rietveld refinement. Therefore, a novel approach combining a hard-sphere approximation model, thermodynamic simulation, thermal expansion measurement and microstructural characterization was developed to assist in a fundamental understanding of the evolution of local composition, lattice parameter, and dendrite volume fraction corresponding to the diffraction data. This methodology yields self-consistent results across different methods. Via this approach, four distinct stages were identified, including: (I) FCC dendrite solidification, (II) solidification of FCC interdendritic region, (III) solid-state interdiffusion and (IV) final cooling with marginal diffusion. It was found out that in Stage I, Cu and Mn were rejected into liquid as Mn35Fe5Co20Ni20Cu20solidified dendritically. During Stage II, the lattice parameter disparity between dendrite and interdendritic region escalated as Cu and Mn continued segregating into the interdendritic region. After complete solidification, during Stage III, the lattice parameter disparity gradually decreases, demonstrating a degree of composition homogenization. The volume fraction of dendrites slightly grewmore »from 58.3 to 65.5%, based on the evolving composition profile across a dendrite/interdendritic interface in diffusion calculations. Postmortem metallography further confirmed that dendrites have a volume fraction of 64.7% ± 5.3% in the final microstructure.

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  5. Abstract

    Hydrogen embrittlement (HE) causes sudden, costly failures of metal components across a wide range of industries. Yet, despite over a century of research, the physical mechanisms of HE are too poorly understood to predict HE-induced failures with confidence. We use non-destructive, synchrotron-based techniques to investigate the relationship between the crystallographic character of grain boundaries and their susceptibility to hydrogen-assisted fracture in a nickel superalloy. Our data lead us to identify a class of grain boundaries with striking resistance to hydrogen-assisted crack propagation: boundaries with low-index planes (BLIPs). BLIPs are boundaries where at least one of the neighboring grains has a low Miller index facet—{001}, {011}, or {111}—along the grain boundary plane. These boundaries deflect propagating cracks, toughening the material and improving its HE resistance. Our finding paves the way to improved predictions of HE based on the density and distribution of BLIPs in metal microstructures.