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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: The Dual Imaging and Diffraction (DIAD) beamline at Diamond Light Source is a new dual-beam instrument for full-field imaging/tomography and powder diffraction. This instrument provides the user community with the capability to dynamically image 2D and 3D complex structures and perform phase identification and/or strain mapping using micro-diffraction. The aim is to enable in situ and in operando experiments that require spatially correlated results from both techniques, by providing measurements from the same specimen location quasi-simultaneously. Using an unusual optical layout, DIAD has two independent beams originating from one source that operate in the medium energy range (7–38 keV) and are combined at one sample position. Here, either radiography or tomography can be performed using monochromatic or pink beam, with a 1.4 mm × 1.2 mm field of view and a feature resolution of 1.2 µm. Micro-diffraction is possible with a variable beam size between 13 µm × 4 µm and 50 µm × 50 µm. One key functionality of the beamline is image-guided diffraction, a setup in which the micro-diffraction beam can be scanned over the complete area of the imaging field-of-view. This moving beam setup enables the collection of location-specific information about the phase composition and/or strains at any given position within the image/tomography field of view. The dual beam design allows fast switching between imaging and diffraction mode without the need of complicated and time-consuming mode switches. Real-time selection of areas of interest for diffraction measurements as well as the simultaneous collection of both imaging and diffraction data of (irreversible) in situ and in operando experiments are possible.

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Abstract: Hard x-ray tomography with Paganin's widespread single-distance phase retrieval filter improves the contrast-to-noise ratio (CNR) while reducing spatial resolution (SR). We demonstrate that a Gaussian filter provided larger CNR at high SR with interpretable density measurements for two medically relevant soft tissue samples. Paganin's filter produced larger CNR at low SR, though a priori assumptions were generally false and image quality gains diminish for CNR > 1. Therefore, simple absorption measurements of low-Z specimens combined with Gaussian filtering can provide improved image quality and model-independent density measurements compared to single-distance phase retrieval.

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Abstract: Advances in high-resolution hard X-ray computed tomography have led to the field of virtual histology to complement histopathological analyses. Phase-contrast modalities have been favored because, for soft tissues, the real part of the refractive index is orders of magnitude greater than the imaginary part. Nevertheless, absorption-contrast measurements of paraffin-embedded tissues have provided exceptionally high contrast combined with a submicron resolution. In this work, we present a quantitative comparison of phase tomography using synchrotron radiation-based X-ray double grating interferometry and conventional synchrotron radiation-based computed tomography in the context of histopathologically relevant paraffin-embedded human brain tissue. We determine the complex refractive index and compare the contrast-to-noise ratio (CNR) of each modality, accounting for the spatial resolution and optimizing the photon energy for absorption tomography. We demonstrate that the CNR in the phase modality is 1.6 times higher than the photon-energy optimized and spatial resolution-matched absorption measurements. We predict, however, that a further optimized phase tomography will provide a CNR gain of 4. This study seeks to boost the discussion of the relative merits of phase and absorption modalities in the context of paraffin-embedded tissues for virtual histology, highlighting the importance of optimization procedures for the two complementary modes and the trade-off between spatial and density resolution, not to mention the disparity in data acquisition and processing.