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Due to their superior fatigue strength, martensitic steels are the material of choice for high cyclic loading applications such as coil springs. However, crack propagation is influenced by residual stresses and their interaction is poorly understood. In fact, linear elastic fracture mechanics predicts unphysical singularities in the strain around the crack tip. In this study, we have combined synchrotron‐based X‐ray diffraction, X‐ray fluorescence and optical microscopy to map the factual strain fields around crack tips with micrometre spatial resolution. X‐ray fluorescence and optical images were co‐registered to locate the crack in the X‐ray diffraction maps. Observed crystal recovery close to cracks confirmed that the diffraction signal originates at least in part from the cracks. The retrieved local strain field around the crack was further improved by averaging information over carefully selected diffraction peaks. This procedure provided strain maps around crack tips with a spatial resolution of about 1 µm and may enable heuristic predictions of further crack growth. Multi‐modal measurements combining X‐ray diffraction, X‐ray fluorescence and optical microscopy allow dynamic crystal recovery effects around martensitic steel crack tips to be studied. The measured strain field around the crack tip shows a significant departure from the predictions of linear elastic fracture mechanics.

X‐ray diffraction with high spatial resolution is commonly used to characterize (poly)crystalline samples with, for example, respect to local strain, residual stress, grain boundaries and texture. However, the investigation of highly absorbing samples or the simultaneous assessment of high‐Z materials by X‐ray fluorescence have been limited due to the utilization of low photon energies. Here, a goniometer‐based setup implemented at the P06 beamline of PETRA III that allows for micrometre spatial resolution with a photon energy of 35 keV and above is reported. A highly focused beam was achieved by using compound refractive lenses, and high‐precision sample manipulation was enabled by a goniometer that allows up to 5D scans (three rotations and two translations). As experimental examples, the determination of local strain variations in martensitic steel samples with micrometre spatial resolution, as well as the simultaneous elemental distribution for high‐Z materials in a thin‐film solar cell, are demonstrated. The proposed approach allows users from the materials‐science community to determine micro‐structural properties even in highly absorbing samples. A demonstration of high‐resolution micro X‐ray diffraction at high photon energies for highly absorbing samples.

To detect faint signals from weakly scattering samples, high-resolution x-ray microscopy typically requires a high photon flux. This exposes samples to high radiation doses and can cause radiation damage. In this work we propose the use of annular optics in scanning microscopy as an alternative to full-aperture optics. Annular optics act as high-pass filters that produce a stronger signal from edges. Compared to regular optics with the same numerical aperture, annular optics expose the sample to less dose while producing the same signal from small sample features. Annular optics benefit significantly from the high photon fluxes of the latest x-ray sources to compensate for their overall smaller cross section. Using numerical simulations, we show that annular optics offer superior optical performance for sample features close to the resolution limit of the optic.

While a few methods for the determination of depth-resolved strain distributions each with inherent limitations are available, tomographic reconstruction has been applied to this problem in only a limited sense. One of the challenges was the potential impact of geometric parallax, which constitutes a non-negligible lateral offset of diffraction information arising from different sample depths at the detector. Here, the effect of parallax was investigated and two main results have emerged. First, the impact of parallax was found to be additive to other offset contributions, which implies a straightforward correction. Second, for tomographic scans utilizing a full 360° rotation parallax has been found to have no impact on reconstructions of angular information.

Ancient Egyptian mummies were often covered with an outer casing, panels and masks made from cartonnage: a lightweight material made from linen, plaster, and recycled papyrus held together with adhesive. Egyptologists, papyrologists, and historians aim to recover and read extant text on the papyrus contained within cartonnage layers, but some methods, such as dissolving mummy casings, are destructive. The use of an advanced range of different imaging modalities was investigated to test the feasibility of non-destructive approaches applied to multi-layered papyrus found in ancient Egyptian mummy cartonnage. Eight different techniques were compared by imaging four synthetic phantoms designed to provide robust, well-understood, yet relevant sample standards using modern papyrus and replica inks. The techniques include optical (multispectral imaging with reflection and transillumination, and optical coherence tomography), X-ray (X-ray fluorescence imaging, X-ray fluorescence spectroscopy, X-ray micro computed tomography and phase contrast X-ray) and terahertz-based approaches. Optical imaging techniques were able to detect inks on all four phantoms, but were unable to significantly penetrate papyrus. X-ray-based techniques were sensitive to iron-based inks with excellent penetration but were not able to detect carbon-based inks. However, using terahertz imaging, it was possible to detect carbon-based inks with good penetration but with less sensitivity to iron-based inks. The phantoms allowed reliable and repeatable tests to be made at multiple sites on three continents. The tests demonstrated that each imaging modality needs to be optimised for this particular application: it is, in general, not sufficient to repurpose an existing device without modification. Furthermore, it is likely that no single imaging technique will to be able to robustly detect and enable the reading of text within ancient Egyptian mummy cartonnage. However, by carefully selecting, optimising and combining techniques, text contained within these fragile and rare artefacts may eventually be open to non-destructive imaging, identification, and interpretation.

Sensitivity to sub-pixel sample features has been demonstrated as a valuable capability of phase contrast x-ray imaging. Here, we report on a method to obtain angular-resolved small angle x-ray scattering distributions with edge-illumination- based imaging utilizing incoherent illumination from an x-ray tube. Our approach provides both the three established image modalities (absorption, differential phase and scatter strength), plus a number of additional contrasts related to unresolved sample features. The complementarity of these contrasts is experimentally validated by using different materials in powder form. As a significant application example we show that the extended complementary contrasts could allow the diagnosis of pulmonary emphysema in a murine model. In support of this, we demonstrate that the properties of the retrieved scattering distributions are consistent with the expectation of increased feature sizes related to pulmonary emphysema. Combined with the simplicity of implementation of edge-illumination, these findings suggest a high potential for exploiting extended sub-pixel contrasts in the diagnosis of lung diseases and beyond.

Faults in vascular (VN) and neuronal networks of spinal cord are responsible for serious neurodegenerative pathologies. Because of inadequate investigation tools, the lacking knowledge of the complete fine structure of VN and neuronal system represents a crucial problem. Conventional 2D imaging yields incomplete spatial coverage leading to possible data misinterpretation, whereas standard 3D computed tomography imaging achieves insufficient resolution and contrast. We show that X-ray high-resolution phase-contrast tomography allows the simultaneous visualization of three-dimensional VN and neuronal systems of ex-vivo mouse spinal cord at scales spanning from millimeters to hundreds of nanometers, with nor contrast agent nor sectioning and neither destructive sample-preparation. We image both the 3D distribution of micro-capillary network and the micrometric nerve fibers, axon-bundles and neuron soma. Our approach is very suitable for pre-clinical investigation of neurodegenerative pathologies and spinal-cord-injuries, in particular to resolve the entangled relationship between VN and neuronal system.

4H Silicon Carbide (4H-SiC) combines many attractive properties such as a high carrier mobility, a wide bandgap, and a high thermal conductivity, making it an ideal candidate for high-power electronic devices. However, a primary challenge in utilizing 4H-SiC is the presence of defects in epitaxial layers, which can significantly degrade device performance. In this study, we have used X-ray transmission topography with a rocking curve imaging technique to characterize the types and distribution of defects in 4H-SiC. Gaussian fitting was applied to the rocking curves, and the resulting maps were used to investigate dislocations in 4H-SiC. Understanding the distribution of the dislocations provides valuable insights into the overall crystal quality, which can guide improvements for the fabrication processes.

The goal of this study was to investigate the performance of 3D synchrotron differential phase contrast (DPC) imaging for the visualization of both macroscopic and microscopic aspects of atherosclerosis in the mouse vasculature ex vivo . The hearts and aortas of 2 atherosclerotic and 2 wild-type control mice were scanned with DPC imaging with an isotropic resolution of 15 μm. The coronary artery vessel walls were segmented in the DPC datasets to assess their thickness and histological staining was performed at the level of atherosclerotic plaques. The DPC imaging allowed for the visualization of complex structures such as the coronary arteries and their branches, the thin fibrous cap of atherosclerotic plaques as well as the chordae tendineae. The coronary vessel wall thickness ranged from 37.4 ± 5.6 μm in proximal coronary arteries to 13.6 ± 3.3 μm in distal branches. No consistent differences in coronary vessel wall thickness were detected between the wild-type and atherosclerotic hearts in this proof-of-concept study, although the standard deviation in the atherosclerotic mice was higher in most segments, consistent with the observation of occasional focal vessel wall thickening. Overall, DPC imaging of the cardiovascular system of the mice allowed for a simultaneous detailed 3D morphological assessment of both large structures and microscopic details.

X-ray ptychography is a cutting edge imaging technique providing ultra-high spatial resolutions. In ptychography, phase retrieval, i.e., the recovery of a complex valued signal from intensity-only measurements, is enabled by exploiting a redundancy of information contained in diffraction patterns measured with overlapping illuminations. For samples that are considerably larger than the probe we show that during the iteration the bulk information has to propagate from the sample edges to the center. This constitutes an inherent limitation of reconstruction speed for algorithms that use a flat initialization. Here, we experimentally demonstrate that a considerable improvement of computational speed can be achieved by utilizing a low resolution sample wavefront retrieved from measured diffraction patterns as initialization. In addition, we show that this approach avoids phase singularity artifacts due to strong phase gradients. Wavefront initialization is computationally fast and compatible with non-bulky samples. Therefore, the presented approach is readily adaptable with established ptychographic reconstruction algorithms implying a wide spread use.