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Abstract: The Dual Imaging and Diffraction (DIAD) beamline at Diamond Light Source (Didcot, U.K.) implements a correlative approach to the dynamic study of materials based on concurrent analysis of identical sample locations using complementary X-ray modalities to reveal structural detail at various length scales. Namely, the underlying beamline principle and its practical implementation allow the collocation of chosen regions within the sample and their interrogation using real-space imaging (radiography and tomography) and reciprocal space scattering (diffraction). The switching between the two principal modes is made smooth and rapid by design, so that the data collected is interlaced to obtain near-simultaneous multimodal characterization. Different specific photon energies are used for each mode, and the interlacing of acquisition steps allows conducting static and dynamic experiments. Building on the demonstrated realization of this state-of-the-art approach requires further refining of the experimental practice, namely, the methods for gauge volume collocation under different modes of beam–sample interaction. To address this challenge, experiments were conducted at DIAD devoted to the study of human dental enamel, a hierarchical structure composed of hydroxyapatite mineral nanocrystals, as a static sample previously affected by dental caries (tooth decay) as well as under dynamic conditions simulating the process of acid demineralization. Collocation and correlation were achieved between WAXS (wide-angle X-ray scattering), 2D (radiographic), and 3D (tomographic) imaging. While X-ray imaging in 2D or 3D modes reveals real-space details of the sample microstructure, X-ray scattering data for each gauge volume provided statistical nanoscale and ultrastructural polycrystal reciprocal-space information such as phase and preferred orientation (texture). Careful registration of the gauge volume positions recorded during the scans allowed direct covisualization of the data from two modalities. Diffraction gauge volumes were identified and visualized within the tomographic data sets, revealing the underlying local information to support the interpretation of the diffraction patterns. The present implementation of the 4D microscopy paradigm allowed following the progression of demineralization and its correlation with time-dependent WAXS pattern evolution in an approach that is transferable to other material systems.

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Abstract: The DIAD beamline for Dual Imaging and Diffraction at Diamond Light Source has opted to use an industrial robot to position its Dectris Pilatus 2M CdTe diffraction detector. This setup was chosen to enable flexible positioning of the detector in a quarter-sphere around the sample position whilst reliably holding the large weight of 139 kg of detector, detector mount and cabling in a stable position. Metrology measurements showed that the detector can be positioned with a linear repeatability of <19.7 µm and a rotational repeatability of <16.3 µrad. The detector position stays stable for a 12 h period with <10.1 µm of movement for linear displacement and <3.8 µrad for rotational displacement. X-ray diffraction from calibration samples confirmed that the robot is sufficiently stable to resolve lattice d-spacings within the instrumental broadening given by detector position and beam divergence.

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Abstract: A primary target towards the clean-up operation of the Fukushima disaster is the retrieval of Molten Core-Concrete Interaction (MCCI) products, presently residing on the basement of the damaged nuclear reactor Units 1–3. MCCI is a fusion of materials, composed of both nuclear fuel cladding and neighbouring structural components. Determining the currently unknown, physical and mechanical properties of MCCI is essential for successful and timely retrieval. In this paper, we aim to experimentally quantify the mechanical properties of a material fabricated to resemble MCCI. A small-scale representative specimen was mechanically tested using Hertzian indentation stepwise loading. Synchrotron X-ray computed tomography was conducted at several loading stages to reveal the sample microstructure and mechanical degradation. The acquired tomograms were analysed by digital volume correlation to measure full-field displacements and strains developed within the sample volume. Young’s modulus and Poisson ratio were determined via this combined methodology.

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Abstract: In this study we investigated the evolution of meso-scale internal stresses and those effects on local deformation behaviour during incremental plastic and creep deformation in type 316H stainless steel at 550°C, using in-situ X-ray synchrotron diffraction and crystal plasticity modelling. Owing to the fast data accusation rate of synchrotron diffraction technique, for the first time, the transient behaviour of different grain families was captured during initial fast stress relaxation period of the displacement-controlled creep dwells. Significantly it is found that the evolution of internal stresses during time independent plastic deformation is distinct from that during time dependent creep deformation. During plastic deformation, lattice strains in the {311} grain family exhibit linear behaviour whereas during creep deformation it exhibits non-linear behaviour, instead the {111} grain family exhibit linear behaviour. A novel unified constitutive law was devised within crystal plasticity framework based on the theoretical physics; the model successfully predicts the macroscopic deformation behaviour as well as the distinction between the evolution of meso-scale internal stresses during plastic and creep deformation, therefore, correctly accounting for the effect of internal stresses generated during plastic deformation on the subsequent creep deformation. The validated model has elucidated the grain-neighbouring effects on individual grain deformations.

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Abstract: Thermal shocks are an important incident in operation of a pressure vessel which can have a significant impact on the structural integrity of the vessel. Often experiments that consider the state of the vessel before and after the thermal shock are used to evaluate the effects of the thermal shock. The studies can be complemented by time-resolved numerical simulations, which may be validated against the final state of the vessel obtained experimentally, to infer the transient response of the material. The transient response is important as the material experiences the highest level of stress in a short period which can induce catastrophic failure. This paper reports time-resolved experimental quantification of strain in reactor pressure vessel material during thermal shock measured by in-situ synchrotron diffraction. Specimens were extracted from a plate of nuclear pressure vessel steel with a nickel alloy cladding deposited by overlay welding. The specimens, with and without cracks, were subjected to thermal loading by heating then rapidly quenching the cladding in cold water. Strains were measured during thermal loading at a point near the crack tip from which the stress state around the crack tip was calculated and compared with a transient finite element model of the experiment. It was found that the peak near-tip stress occurred within the first second after the onset of rapid cooling. It was demonstrated from experimental measurements that the peak stress intensity factor occurred during thermal shock, rather than under steady conditions before or after the thermal shock. It was shown that although the finite element simulation predicts the steady state condition of the material after thermal shock, its transient response dependents significantly on a number of inputs with high uncertainty, making its time-resolved results unreliable for high-fidelity integrity assessments.