X-ray diffraction contrast tomography ͑DCT͒ is a technique for mapping grain shape and orientation in plastically undeformed polycrystals. In this paper, we describe a modified DCT data acquisition strategy which permits the incorporation of an innovative Friedel pair method for analyzing diffraction data. Diffraction spots are acquired during a 360°rotation of the sample and are analyzed in terms of the Friedel pairs ͑͑hkl͒ and ͑hkl͒ reflections, observed 180°apart in rotation͒. The resulting increase in the accuracy with which the diffraction vectors are determined allows the use of improved algorithms for grain indexing ͑assigning diffraction spots to the grains from which they arise͒ and reconstruction. The accuracy of the resulting grain maps is quantified with reference to synchrotron microtomography data for a specimen made from a beta titanium system in which a second phase can be precipitated at grain boundaries, thereby revealing the grain shapes. The simple changes introduced to the DCT methodology are equally applicable to other variants of grain mapping.

X-ray diffraction contrast tomography is a recently developed, non-destructive synchrotron imaging technique which characterizes microstructure and grain orientation in polycrystalline materials in three dimensions. By combining it with propagation-based phasecontrast tomography it is possible to get a full picture description for the analysis of local crack growth rate of short fatigue cracks in three dimensions: the three-dimensional crack morphology at different propagation stages, and the shape and orientation of the grains around the crack. An approach has been developed on the metastable beta titanium alloy Ti 21S that allows for visualization and analysis of the growth rate and crystallographic orientation of the fracture surface.

Diffraction contrast tomography is a near‐field diffraction‐based imaging technique that provides high‐resolution grain maps of polycrystalline materials simultaneously with the orientation and average elastic strain tensor components of the individual grains with an accuracy of a few times 10−4. Recent improvements that have been introduced into the data analysis are described. The ability to process data from arbitrary detector positions allows for optimization of the experimental setup for higher spatial or strain resolution, including high Bragg angles (0 < 2θ < 180°). The geometry refinement, grain indexing and strain analysis are based on Friedel pairs of diffraction spots and can handle thousands of grains in single‐ or multiphase materials. The grain reconstruction is performed with a simultaneous iterative reconstruction technique using three‐dimensional oblique angle projections and GPU acceleration. The improvements are demonstrated with the following experimental examples: (1) uranium oxide mapped at high spatial resolution (300 nm voxel size); (2) combined grain mapping and section topography at high Bragg angles of an Al–Li alloy; (3) ferrite and austenite crystals in a dual‐phase steel; (4) grain mapping and elastic strains of a commercially pure titanium sample containing 1755 grains.

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The first results of three-dimensional grain mapping using a laboratory tomograph equipped with a microfocus W target X-ray tube source, operated at 90 kV and 350 mA, are presented. Adapted algorithms exploit the polychromatic radiation spectrum and the projection magnification arising from the cone-beam geometry. The first map of grain shapes and crystallographic orientations from a titanium sample containing 42 grains is presented and its validity confirmed by a phase contrast reconstruction of the grain boundaries. Perspectives are given for the further development of the technique to accommodate samples with more grains or with greater intragranular orientation spread.

The ability to characterise crystallographic microstructure, non-destructively and in three-dimensions, is a powerful tool for understanding many aspects related to damage and deformation mechanisms in polycrystalline materials. To this end, the technique of X-ray diffraction contrast tomography (DCT) using monochromatic synchrotron and polychromatic laboratory X-ray sources has been shown to be capable of mapping crystal grains and their orientations non-destructively in 3D. Here we describe a novel laboratory-based X-ray DCT modality (LabDCT), enabling the wider accessibility of the DCT technique for routine use and in-depth studies of, for example, temporal changes in crystallographic grain structure non-destructively over time through ‘4D’ in situ time-lapse studies. The capability of the technique is demonstrated by studying a titanium alloy (Ti-β21S) sample. In the current implementation the smallest grains that can be reliably detected are around 40 μm. The individual grain locations and orientations are reconstructed using the LabDCT method and the results are validated against independent measurements from phase contrast tomography and electron backscatter diffraction respectively. Application of the technique promises to provide important insights related to the roles of recrystallization and grain growth on materials properties as well as supporting 3D polycrystalline modelling of materials performance.

Pressureless sintering of loose or compacted granular bodies at elevated temperature occurs by a combination of particle rearrangement, rotation, local deformation and diffusion, and grain growth. Understanding of how each of these processes contributes to the densification of a powder body is still immature. Here we report a fundamental study coupling the crystallographic imaging capability of laboratory diffraction contrast tomography (LabDCT) with conventional computed tomography (CT) in a time-lapse study. We are able to follow and differentiate these processes non-destructively and in three-dimensions during the sintering of a simple copper powder sample at 1050 °C. LabDCT quantifies particle rotation (to <0.05° accuracy) and grain growth while absorption CT simultaneously records the diffusion and deformation-related morphological changes of the sintering particles. We find that the rate of particle rotation is lowest for the more highly coordinated particles and decreases during sintering. Consequently, rotations are greater for surface breaking particles than for more highly coordinated interior ones. Both rolling (cooperative) and sliding particle rotations are observed. By tracking individual grains the grain growth/shrinkage kinetics during sintering are quantified grain by grain for the first time. Rapid, abnormal grain growth is observed for one grain while others either grow or are consumed more gradually.

X-ray radiography is a common tool in the study of old master paintings. Transmission imaging can visualize hidden paint layers as well as the structure of the panel or canvas. In some medieval altarpieces, relics seem to have been imbedded in the wooden carrier of paintings. These are most probably thin organic fibrous materials such as paper or textile, which in traditional radiography are shadowed by the more absorbing surrounding material. This paper studies the application potential of synchrotron-based tomographic and laminographic imaging complemented with phase-contrast imaging for detection of such relics. The techniques are applied to a dummy painting. The results demonstrate that by using these imaging methods it is possible to threedimensionally visualize hidden cavities in panels and detect thin fibrous low-Z materials sandwiched between a high-Z paint layer and a thick wooden panel.