Hierarchically guided in situ nanolaminography for the visualisation of damage nucleation in alloy sheets.

Hierarchical guidance is developed for three-dimensional (3D) nanoscale X-ray imaging, enabling identification, refinement, and tracking of regions of interest (ROIs) within specimens considerably exceeding the field of view. This opens up new possibilities for in situ investigations. Experimentally, the approach takes advantage of rapid multiscale measurements based on magnified projection microscopy featuring continuous zoom capabilities. Immediate and continuous feedback on the subsequent experimental progress is enabled by suitable on-the-fly data processing. For this, by theoretical justification and experimental validation, so-called quasi-particle phase-retrieval is generalised to conical-beam conditions, being key for sufficiently fast computation without significant loss of imaging quality and resolution compared to common approaches for holographic microscopy. Exploiting 3D laminography, particularly suited for imaging of ROIs in laterally extended plate-like samples, the potential of hierarchical guidance is demonstrated by the in situ investigation of damage nucleation inside alloy sheets under engineering-relevant boundary conditions, providing novel insight into the nanoscale morphological development of void and particle clusters under mechanical load. Combined with digital volume correlation, we study deformation kinematics with unprecedented spatial resolution. Correlation of mesoscale (i.e. strain fields) and nanoscale (i.e. particle cracking) evolution opens new routes for the understanding of damage nucleation within sheet materials with application-relevant dimensions.

High-resolution neutron imaging of salt precipitation and water transport in zero-gap CO2 electrolysis.

The electrochemical reduction of CO2 is a pivotal technology for the defossilization of the chemical industry. Although pilot-scale electrolyzers exist, water management and salt precipitation remain a major hurdle to long-term operation. In this work, we present high-resolution neutron imaging (6 µm) of a zero-gap CO2 electrolyzer to uncover water distribution and salt precipitation under application-relevant operating conditions (200 mA cm-2 at a cell voltage of 2.8 V with a Faraday efficiency for CO of 99%). Precipitated salts penetrating the cathode gas diffusion layer can be observed, which are believed to block the CO2 gas transport and are therefore the major cause for the commonly observed decay in Faraday efficiency. Neutron imaging further shows higher salt accumulation under the cathode channel of the flow field compared to the land.

Water management in anion-exchange membrane water electrolyzers under dry cathode operation.

Dry cathode operation is a desired operation mode in anion-exchange membrane water electrolyzers to minimize contamination of the generated hydrogen. However, water management under such operation conditions makes it challenging to maintain reliable performance and durability. Here, we utilize high-resolution in situ neutron imaging (∼6 µm effective resolution) to analyze the water content inside the membrane-electrode-assembly of an anion-exchange membrane water electrolyzer. The ion-exchange capacity (IEC) and thus hydrophilicity of the polymer binder in the cathode catalyst layer is varied to study the influence on water content in the anode (mid IEC, 1.8-2.2 meq. g-1 and high IEC, 2.3-2.6 meq. g-1). The neutron radiographies show that a higher ion-exchange capacity binder allows improved water retention, which reduces the drying-out of the cathode at high current densities. Electrochemical measurements confirm a generally better efficiency for a high IEC cell above 600 mA cm-2. At 1.5 A cm-2 the high IEC has a 100 mV lower overpotential (2.1 V vs. 2.2 V) and a lower high frequency resistance (210 mΩ cm-2 vs. 255 mΩ cm-2), which is believed to be linked to the improved cathode water retention and membrane humidification. As a consequence, the performance stability of the high IEC cell at 1 A cm-2 is also significantly better than that of the mid IEC cell (45 mV h-1 vs. 75 mV h-1).

The Hydration State of Bone Tissue Affects Contrast in Neutron Tomographic Images.

Neutron tomography has emerged as a promising imaging technique for specific applications in bone research. Neutrons have a strong interaction with hydrogen, which is abundant in biological tissues, and they can penetrate through dense materials such as metallic implants. However, in addition to long imaging times, two factors have led to challenges in running in situ mechanical characterization experiments on bone tissue using neutron tomography: 1) the high water content in specimens reduces the visibility of internal trabecular structures; 2) the mechanical properties of bone are dependent on the hydration state of the tissue, with drying being reported to cause increased stiffness and brittleness. This study investigates the possibility of improving image quality in terms of neutron transmission and contrast between material phases by drying and rehydrating in heavy water. Rat tibiae and trabecular bovine bone plugs were imaged with neutron tomography at different hydration states and mechanical testing of the bone plugs was carried out to assess effects of drying and rehydration on the mechanical properties of bone. From analysis of image histograms, it was found that drying reduced the contrast between bone and soft tissue, but the contrast was restored with rehydration. Contrast-to-noise ratios and line profiles revealed that the contrast between bone tissue and background was reduced with increasing rehydration duration but remained sufficient for identifying internal structures as long as no free liquid was present inside the specimen. The mechanical analysis indicated that the proposed fluid exchange protocol had no adverse effects on the mechanical properties.

The scale of a martian hydrothermal system explored using combined neutron and x-ray tomography.

Nakhlite meteorites are igneous rocks from Mars that were aqueously altered ~630 million years ago. Hydrothermal systems on Earth are known to provide microhabitats; knowledge of the extent and duration of these systems is crucial to establish whether they could sustain life elsewhere in the Solar System. Here, we explore the three-dimensional distribution of hydrous phases within the Miller Range 03346 nakhlite meteorite using nondestructive neutron and x-ray tomography to determine whether alteration is interconnected and pervasive. The results reveal discrete clusters of hydrous phases within and surrounding olivine grains, with limited interconnectivity between clusters. This implies that the fluid was localized and originated from the melting of local subsurface ice following an impact event. Consequently, the duration of the hydrous alteration was likely short, meaning that the martian crust sampled by the nakhlites could not have provided habitable environments that could harbor any life on Mars during the Amazonian.

Tofu: a fast, versatile and user-friendly image processing toolkit for computed tomography.

Tofu is a toolkit for processing large amounts of images and for tomographic reconstruction. Complex image processing tasks are organized as workflows of individual processing steps. The toolkit is able to reconstruct parallel and cone beam as well as tomographic and laminographic geometries. Many pre- and post-processing algorithms needed for high-quality 3D reconstruction are available, e.g. phase retrieval, ring removal and de-noising. Tofu is optimized for stand-alone GPU workstations on which it achieves reconstruction speed comparable with costly CPU clusters. It automatically utilizes all GPUs in the system and generates 3D reconstruction code with minimal number of instructions given the input geometry (parallel/cone beam, tomography/laminography), hence yielding optimal run-time performance. In order to improve accessibility for researchers with no previous knowledge of programming, tofu contains graphical user interfaces for both optimization of 3D reconstruction parameters and batch processing of data with pre-configured workflows for typical computed tomography reconstruction. The toolkit is open source and extensive documentation is available for both end-users and developers. Thanks to the mentioned features, tofu is suitable for both expert users with specialized image processing needs (e.g. when dealing with data from custom-built computed tomography scanners) and for application-specific end-users who just need to reconstruct their data on off-the-shelf hardware.

Compact and versatile neutron imaging detector with sub-4µm spatial resolution based on a single-crystal thin-film scintillator.

A large and increasing number of scientific domains pushes for high neutron imaging resolution achieved in reasonable times. Here we present the principle, design and performance of a detector based on infinity corrected optics combined with a crystalline Gd3Ga5O12 : Eu scintillator, which provides an isotropic sub-4 µm true resolution. The exposure times are only of a few minutes per image. This is made possible also by the uniquely intense cold neutron flux available at the imaging beamline NeXT-Grenoble. These comparatively rapid acquisitions are compatible with multiple high quality tomographic acquisitions, opening new venues for in-operando testing, as briefly exemplified here.

Heterogeneity of the osteocyte lacuno-canalicular network architecture and material characteristics across different tissue types in healing bone.

Various tissue types, including fibrous connective tissue, bone marrow, cartilage, woven and lamellar bone, coexist in healing bone. Similar to most bone tissue type, healing bone contains a lacuno-canalicular network (LCN) housing osteocytes. These cells are known to orchestrate bone remodeling in healthy bone by sensing mechanical strains and translating them into biochemical signals. The structure of the LCN is hypothesized to influence mineralization processes. Hence, the aim of the present study was to visualize and match spatial variations in the LCN topology with mineral characteristics, within and at the interfaces of the different tissue types that comprise healing bone. We applied a correlative multi-method approach to visualize the LCN architecture and quantify mineral particle size and orientation within healing femoral bone in a mouse osteotomy model (26 weeks old C57BL/6 mice). This approach revealed structural differences across several length scales during endochondral ossification within the following regions: calcified cartilage, bony callus, cortical bone and a transition zone between the cortical and callus region analyzed 21 days after the osteotomy. In this transition zone, we observed a continuous convergence of mineral characteristics and osteocyte lacunae shape as well as discontinuities in the lacunae volume and LCN connectivity. The bony callus exhibits a 34% higher lacunae number density and 40% larger lacunar volume compared to cortical bone. The presented correlations between LCN architecture and mineral characteristics improves our understanding of how bone develops during healing and may indicate a contribution of osteocytes to bone (re)modeling.

Multi-scale quantification and modeling of aged nanostructured silicon-based composite anodes.

Advanced anode material designs utilizing dual phase alloy systems like Si/FeSi2 nano-composites show great potential to decrease the capacity degrading and improve the cycling capability for Lithium (Li)-ion batteries. Here, we present a multi-scale characterization approach to understand the (de-)lithiation and irreversible volumetric changes of the amorphous silicon (a-Si)/crystalline iron-silicide (c-FeSi2) nanoscale phase and its evolution due to cycling, as well as their impact on the proximate pore network. Scattering and 2D/3D imaging techniques are applied to probe the anode structural ageing from nm to µm length scales, after up to 300 charge-discharge cycles, and combined with modeling using the collected image data as an input. We obtain a quantified insight into the inhomogeneous lithiation of the active material induced by the morphology changes due to cycling. The electrochemical performance of Li-ion batteries does not only depend on the active material used, but also on the architecture of its proximity.

Influence of loading condition and anatomical location on human cortical bone linear micro-cracks.

Human cortical bone fracture toughness depends on the anatomical locations under quasi-static loading. Recent results also showed that under fall-like loading, cortical bone fracture toughness is similar at different anatomical locations in the same donor. While cortical bone toughening mechanisms are known to be dependent on the tissue architecture under quasi-static loading, the fracture mechanisms during a fall are less studied. In the current study, the structural parameters of eight paired femoral diaphyses, femoral necks and radial diaphyses were mechanically tested under quasi-static and fall-like loading conditions (female donors, 70 ±â€¯14 y.o., [50-91 y.o.]). Synchrotron radiation micro-CT imaging was used to quantify the amount of micro-cracks formed during loading. The volume fraction of these micro-cracks was significantly higher within the specimens loaded under a quasi-static condition than under a loading representative of a fall. Under fall-like loading, there was no difference in crack volume fraction between the different paired anatomical locations. This result shows that the micro-cracking toughening mechanism depends both on the anatomical location and on the loading condition.

3D micro structural analysis of human cortical bone in paired femoral diaphysis, femoral neck and radial diaphysis.

Human bone is known to adapt to its mechanical environment in a living body. Both its architecture and microstructure may differ between weight-bearing and non-weight-bearing bones. The aim of the current study was to analyze in three dimensions, the morphology of the multi-scale porosities on human cortical bone at different locations. Eight paired femoral diaphyses, femoral necks, and radial diaphyses were imaged using Synchrotron Radiation µCT with a 0.7 µm isotropic voxel size. The spatial resolution facilitates the investigation of the multiscale porosities of cortical bone, from the osteonal canals system down to the osteocyte lacunar system. Our results showed significant differences in the microstructural properties, regarding both osteonal canals and osteocytes lacunae, between the different anatomical locations. The radius presents significantly lower osteonal canal volume fraction and smaller osteonal canals than the femoral diaphysis or neck. Osteocytes lacunae observed in the radius are significantly different in shape than in the femur, and lacunar density is higher in the femoral neck. These results show that the radius, a non-weight-bearing bone, is significantly different in terms of its microstructure from a weight-bearing bone such as the femur. This implies that the cortical bone properties evaluated on the femoral diaphysis, the main location studied within the literature, cannot be generalized to other anatomical locations.

Electromigration Mechanism of Failure in Flip-Chip Solder Joints Based on Discrete Void Formation.

In this investigation, SnAgCu and SN100C solders were electromigration (EM) tested, and the 3D laminography imaging technique was employed for in-situ observation of the microstructure evolution during testing. We found that discrete voids nucleate, grow and coalesce along the intermetallic compound/solder interface during EM testing. A systematic analysis yields quantitative information on the number, volume, and growth rate of voids, and the EM parameter of DZ*. We observe that fast intrinsic diffusion in SnAgCu solder causes void growth and coalescence, while in the SN100C solder this coalescence was not significant. To deduce the current density distribution, finite-element models were constructed on the basis of the laminography images. The discrete voids do not change the global current density distribution, but they induce the local current crowding around the voids: this local current crowding enhances the lateral void growth and coalescence. The correlation between the current density and the probability of void formation indicates that a threshold current density exists for the activation of void formation. There is a significant increase in the probability of void formation when the current density exceeds half of the maximum value.

Real-time image-content-based beamline control for smart 4D X-ray imaging.

Real-time processing of X-ray image data acquired at synchrotron radiation facilities allows for smart high-speed experiments. This includes workflows covering parameterized and image-based feedback-driven control up to the final storage of raw and processed data. Nevertheless, there is presently no system that supports an efficient construction of such experiment workflows in a scalable way. Thus, here an architecture based on a high-level control system that manages low-level data acquisition, data processing and device changes is described. This system is suitable for routine as well as prototypical experiments, and provides specialized building blocks to conduct four-dimensional in situ, in vivo and operando tomography and laminography.

Melanosomes in pigmented epithelia maintain eye lens transparency during zebrafish embryonic development.

Altered levels of trace elements are associated with increased oxidative stress that is eventually responsible for pathologic conditions. Oxidative stress has been proposed to be involved in eye diseases, including cataract formation. We visualized the distribution of metals and other trace elements in the eye of zebrafish embryos by micro X-ray fluorescence (µ-XRF) imaging. Many elements showed highest accumulation in the retinal pigment epithelium (RPE) of the zebrafish embryo. Knockdown of the zebrafish brown locus homologues tyrp1a/b eliminated accumulation of these elements in the RPE, indicating that they are bound by mature melanosomes. Furthermore, albino (slc45a2) mutants, which completely lack melanosomes, developed abnormal lens reflections similar to the congenital cataract caused by mutation of the myosin chaperon Unc45b, and an in situ spin trapping assay revealed increased oxidative stress in the lens of albino mutants. Finally transplanting a wildtype lens into an albino mutant background resulted in cataract formation. These data suggest that melanosomes in pigment epithelial cells protect the lens from oxidative stress during embryonic development, likely by buffering trace elements.

Direct Fourier Inversion Reconstruction Algorithm for Computed Laminography.

Synchrotron radiation computed laminography (CL) was developed to complement the conventional computed tomography as a non-destructive 3D imaging method for the inspection of flat thin objects. Recent progress in hardware at synchrotron sources allows one to record internal evolution of specimens at the micrometer scale and sub-second range but also requires increased reconstruction speed to follow structural changes online. A 3D image of the sample interior is usually reconstructed by the well-established filtered backprojection (FBP) approach. Despite of a great success in the reduction of reconstruction time via parallel computations, the FBP algorithm still remains a time-consuming procedure. A promising way to significantly shorten computation time is to directly perform backprojection in frequency domain (a direct Fourier inversion approach). The corresponding algorithms are rarely considered in the literature because of a poor performance or inferior reconstruction quality resulted from inaccurate interpolation in Fourier domain. In this paper, we derive a Fourier-based reconstruction equation designed for the CL scanning geometry. Furthermore, we outline the translation of the continuous solution to a discrete version, which utilizes 3D sinc interpolation. A projection resampling technique allowing for the reduction of the expensive interpolation to its 1D version is proposed. A series of numerical experiments confirms that the resulting image quality is well comparable with the FBP approach while reconstruction time is drastically reduced.

Gauging low-dose X-ray phase-contrast imaging at a single and large propagation distance.

The interactions of a beam of hard and spatio-temporally coherent X-rays with a soft-matter sample primarily induce a transverse distribution of exit phase variations δϕ (retardations or advancements in pieces of the wave front exiting the object compared to the incoming wave front) whose free-space propagation over a distance z gives rise to intensity contrast gz. For single-distance image detection and |δϕ| ≪ 1 all-order-in-z phase-intensity contrast transfer is linear in δϕ. Here we show that ideal coherence implies a decay of the (shot-)noise-to-signal ratio in gz and of the associated phase noise as z(-1/2) and z(-1), respectively. Limits on X-ray dose thus favor large values of z. We discuss how a phase-scaling symmetry, exact in the limit δϕ → 0 and dynamically unbroken up to |δϕ| ∼ 1, suggests a filtering of gz in Fourier space, preserving non-iterative quasi-linear phase retrieval for phase variations up to order unity if induced by multi-scale objects inducing phase variations δϕ of a broad spatial frequency spectrum. Such an approach continues to be applicable under an assumed phase-attenuation duality. Using synchrotron radiation, ex and in vivo microtomography on frog embryos exemplifies improved resolution compared to a conventional single-distance phase-retrieval algorithm.

Three-dimensional microscale modelling of CO2 transport and light propagation in tomato leaves enlightens photosynthesis.

We present a combined three-dimensional (3-D) model of light propagation, CO2 diffusion and photosynthesis in tomato (Solanum lycopersicum L.) leaves. The model incorporates a geometrical representation of the actual leaf microstructure that we obtained with synchrotron radiation X-ray laminography, and was evaluated using measurements of gas exchange and leaf optical properties. The combination of the 3-D microstructure of leaf tissue and chloroplast movement induced by changes in light intensity affects the simulated CO2 transport within the leaf. The model predicts extensive reassimilation of CO2 produced by respiration and photorespiration. Simulations also suggest that carbonic anhydrase could enhance photosynthesis at low CO2 levels but had little impact on photosynthesis at high CO2 levels. The model confirms that scaling of photosynthetic capacity with absorbed light would improve efficiency of CO2 fixation in the leaf, especially at low light intensity.

Synchrotron X-ray computed laminography of the three-dimensional anatomy of tomato leaves.

Synchrotron radiation computed laminography (SR-CL) is presented as an imaging method for analyzing the three-dimensional (3D) anatomy of leaves. The SR-CL method was used to provide 3D images of 1-mm² samples of intact leaves at a pixel resolution of 750 nm. The method allowed visualization and quantitative analysis of palisade and spongy mesophyll cells, and showed local venation patterns, aspects of xylem vascular structure and stomata. The method failed to image subcellular organelles such as chloroplasts. We constructed 3D computer models of leaves that can provide a basis for calculating gas exchange, light penetration and water and solute transport. The leaf anatomy of two different tomato genotypes grown in saturating light conditions was compared by 3D analysis. Differences were found in calculated values of tissue porosity, cell number density, cell area to volume ratio and cell volume and cell shape distributions of palisade and spongy cell layers. In contrast, the exposed cell area to leaf area ratio in mesophyll, a descriptor that correlates to the maximum rate of photosynthesis in saturated light conditions, was no different between spongy and palisade cells or between genotypes. The use of 3D image processing avoids many of the limitations of anatomical analysis with two-dimensional sections.

Direct three-dimensional imaging of polymer-water interfaces by nanoscale hard X-ray phase tomography.

We report three-dimensional (3D) direct imaging of complex surface-liquid interfaces by hard X-ray phase contrast tomography as a non-destructive approach for the morphological characterization of surfaces at the micro- and nanoscale in contact with water. Specifically, we apply this method to study the solid-air-water interface in hydrophobic macroporous polymethacrylate surfaces, and the solid-oil-water interface in slippery liquid-infused porous surfaces (SLIPS). Varying the isotropic spatial resolution allows the 3D quantitative characterization of individual polymer globules, globular clusters (porosity) as well as the infused lubricant layer on SLIPS. Surface defects were resolved at the globular level. We show the first application of X-ray nanotomography to hydrated surface characterizations and we anticipate that X-ray nanoscale imaging will open new ways for various surface/interface studies.

Efficient volume reconstruction for parallel-beam computed laminography by filtered backprojection on multi-core clusters.

Computed laminography (CL) was developed to use X-rays from synchrotron sources for high-resolution imaging of the internal structure of a flat specimen from a series of 2-D projection images. The projections are acquired by irradiation of the sample under different rotation angles where the object rotation axis is inclined with respect to the beam direction. This yields for laterally extended objects a more uniform average transmitted intensity during sample rotation compared with computed tomography (CT). The reconstruction problem of CL cannot be reduced to a data-efficient 2-D case (as for parallel-beam CT) since each single slice perpendicular to the rotation axis requires a 2-D region on the detector as input data for all projection directions. This paper describes a computationally efficient reconstruction procedure based on filtered backprojection (FBP) adapted to the CL acquisition geometry. From the Fourier slice theorem, we derive a framework for analytic image reconstruction and outline implementation details of the generic FBP algorithm. Different approaches reducing the reconstruction time by means of parallel and distributed computations are considered and evaluated.