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Abstract: The crystallographic texture development during processing of dual-phase Ti alloys like Ti-6Al-4 V is of fundamental technological importance. However, measuring texture in both phases in these materials is a significant challenge because of the spatial inhomogeneity of the texture and low volume fraction of the minority β-phase at room temperature. Here we demonstrate how synchrotron X-ray diffraction can be used to overcome these difficulties and measure texture and texture variation in hot-rolled samples in a reproducible manner. The texture in hot-rolled Ti-64 was calculated from 2D synchrotron diffraction patterns obtained along different directions. The data was analysed using MAUD, which is based on Rietveld refinement of the diffracted intensities, and using a Fourier series based analysis method, that extracts intensities directly from the 2D diffraction patterns, and then uses the open-source software MTEX to fit an orientation distribution function (ODF). By comparing the results with faithful EBSD measurements, we show that the Fourier series method produces much more accurate texture measurements, especially for the minority β-phase. We also show that a minimum of 2, and preferably 3, different measurement orientations are needed to fully represent the texture. This implies that measurements of texture which rely on diffraction data from a single sample orientation, like in fast in-situ studies or spatially resolved measurements, can only provide qualitative information and must be interpreted with care.

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Abstract: Deformation bands, or tabular zones of localised strain, are a common manifestation of deformation in upper crustal sedimentary rocks. Any mining or energy-related engineering applications must consider the possibility of reactivating these pre-existing failure planes because doing so can cause seismicity and compartmentalise the reservoir. However, there has only been a small amount of research done on laboratory-induced deformation in rocks with natural deformation features. On a low porosity bioclastic calcarenite from the Cotiella Basin, Spanish Pyrenees, our current experimental work aims to capture, for the first time to our knowledge, the dominant failure mechanisms during the reactivation of natural deformation bands oriented at different angles to the principal stress direction. At the I12-JEEP beamline at the synchrotron facility of Diamond Light Source, UK, we carried out triaxial compression experiments using a modified version of the Mjolnir cell used by Cartwright-Taylor et al., (2022) to examine how these highly heterogeneous rocks respond to additional mechanical deformation. During the deformation experiments, 4D (time and space) x-ray tomography images (8 m voxel size resolution) were acquired. We tested confining pressures between 10 MPa and 30 MPa. The mechanical data demonstrate that the existence of natural deformation features within the tested samples weakens the material. For instance, solid samples of the host rock subjected to the same confining pressures had higher peak differential stresses. Additionally, our findings demonstrate that new deformation bands form as their angle, θ, to σ1 increases, while the reactivation of pre-exiting deformation bands in this low porosity carbonate only occurs for dipping angles close to 70o. The spatio-temporal relationships between the naturally occurring and laboratory-induced deformation bands and fractures were investigated using time-resolved x-ray tomography and Digital Volume Correlation (DVC). Volumetric and shear strain fields were calculated using the SPAM software (Stamati et al., 2020). The orientation of the recently formed failure planes is influenced by the orientation of the pre-existing bands, as well as their width and the presence (or absence) of porosity along their length. Additionally, pre-existing secondary deformation features found in the tested material trigger additional mechanical damage that either promotes the development or deflects the new failure planes.

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Abstract: A supersaturated  phase microstructure is produced in Ni-based superalloys using laser powder bed fusion (L-PBF) – the cooling rate arising from the process is shown to suppress the solid-state precipitation of the  phase. The response of the material to a heat treatment therefore requires new understanding at the fundamental level, since the first population of  precipitate forms upon heating, in contrast to cooling from homogenisation above the  solvus. Here, we have interrogated two new nickel-based superalloys designed for the L-PBF technology, both in situ and ex situ, at multiple length scales using advanced characterisation methods. First, we conducted in situ synchrotron X-ray diffraction during various heat treatments to trace the evolution of the  volume fraction with temperature. The first structural changes were detected at an unexpectedly low temperature of 445 °C. Second, the temperature for  nucleation and its sensitivity to heating rate was studied using an electrical resistivity method. Then, the  composition upon heating, isothermal holding and cooling is analysed using atom probe tomography (APT), the result is rationalised by further scanning-transmission electron microscopy and nanoscale secondary ion mass spectroscopy. Finally, static recrystallisation during isothermal exposure was investigated, which occurs within minutes. This work sheds light on a new strategy of tailoring microstructure for additively manufactured superalloys by manipulation of the  precipitate distribution upon heating.

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Abstract: Short range order and topology of GexS100-x glasses over a broad composition range (20 ≤ x ≤ 42 in at%) was investigated by neutron diffraction, X-ray diffraction, and Ge K-edge extended X-ray absorption fine structure (EXAFS) measurements. The experimental data sets were fitted simultaneously in the framework of the reverse Monte Carlo simulation method. It was found that both constituents (Ge and S) satisfy the Mott-rule in all investigated glasses: Ge and S atoms have 4 and 2 neighbours, respectively. The structure of these glasses can be described with the chemically ordered network model: Ge-S bonds are preferred; S-S bonds are present only in S-rich glasses. Dedicated simulations showed that Ge-Ge bonds are necessary in Ge-rich glasses. Connections between Ge atoms (such as edge-sharing GeS4/2 tetrahedra) in stoichiometric and S-rich glasses were analysed. The frequency of primitive rings was also calculated.

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Abstract: Three-dimensional X-ray diffraction (3DXRD) is shown to be feasible at the I12 Joint Engineering, Environmental and Processing (JEEP) beamline of Diamond Light Source. As a demonstration, a microstructually simple low-carbon ferritic steel was studied in a highly textured and annealed state. A processing pipeline suited to this beamline was created, using software already established in the 3DXRD user community, enabling grain centre-of-mass positions, orientations and strain tensor elements to be determined. Orientations, with texture measurements independently validated from electron backscatter diffraction (EBSD) data, possessed a ∼0.1° uncertainty, comparable with other 3DXRD instruments. The spatial resolution was limited by the far-field detector pixel size; the average of the grain centre of mass position errors was determined as ±∼80 µm. An average per-grain error of ∼1 × 10−3 for the elastic strains was also measured; this could be reduced in future experiments by improving sample preparation, geometry calibration, data collection and analysis techniques. Application of 3DXRD onto I12 shows great potential, where its implementation is highly desirable due to the flexible, open architecture of the beamline. User-owned or designed sample environments can be used, thus 3DXRD could be applied to previously unexplored scientific areas.