Development towards high-resolution kHz-speed rotation-free volumetric imaging.

X-ray multi-projection imaging (XMPI) has the potential to provide rotation-free 3D movies of optically opaque samples. The absence of rotation enables superior imaging speed and preserves fragile sample dynamics by avoiding the centrifugal forces introduced by conventional rotary tomography. Here, we present our XMPI observations at the ID19 beamline (ESRF, France) of 3D dynamics in melted aluminum with 1000 frames per second and 8 µm resolution per projection using the full dynamical range of our detectors. Since XMPI is a method under development, we also provide different tests for the instrumentation of up to 3000 frames per second. As the high-brilliance of 4th generation light-sources becomes more available, XMPI is a promising technique for current and future X-ray imaging instruments.

An efficient system matrix factorization method for scanning diffraction based strain tensor tomography.

Diffraction-based tomographic strain tensor reconstruction problems in which a strain tensor field is determined from measurements made in different crystallographic directions are considered in the context of sparse matrix algebra. Previous work has shown that the estimation of the crystal elastic strain field can be cast as a linear regression problem featuring a computationally involved assembly of a system matrix forward operator. This operator models the perturbation in diffraction signal as a function of spatial strain tensor state. The structure of this system matrix is analysed and a block-partitioned factorization is derived that reveals the forward operator as a sum of weighted scalar projection operators. Moreover, the factorization method is generalized for another diffraction model in which strain and orientation are coupled and can be reconstructed jointly. The proposed block-partitioned factorization method provides a bridge to classical absorption tomography and allows exploitation of standard tomographic ray-tracing libraries for implementation of the forward operator and its adjoint. Consequently, RAM-efficient, GPU-accelerated, on-the-fly strain/orientation tensor reconstruction is made possible, paving the way for higher spatial resolution studies of intragranular deformation.

xrd_simulator: 3D X-ray diffraction simulation software supporting 3D polycrystalline microstructure morphology descriptions.

An open source Python package named xrd_simulator, capable of simulating geometrical interactions between a monochromatic X-ray beam and a polycrystalline microstructure, is described and demonstrated. The software can simulate arbitrary intragranular lattice variations of single crystals embedded within a multiphase 3D aggregate by making use of a tetrahedral mesh representation where each element holds an independent lattice. By approximating the X-ray beam as an arbitrary convex polyhedral region in space and letting the sample be moved continuously through arbitrary rigid motions, data from standard and non-standard measurement sequences can be simulated. This implementation is made possible through analytical solutions to a modified, time-dependent version of the Laue equations. The software, which primarily targets three-dimensional X-ray diffraction microscopy (high-energy X-ray diffraction microscopy) type experiments, enables the numerical exploration of which sample quantities can and cannot be reconstructed for a given acquisition scheme. Similarly, xrd_simulator targets investigations of different measurement sequences in relation to optimizing both experimental run times and sampling.

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.

Quantifying local rearrangements in three-dimensional granular materials: Rearrangement measures, correlations, and relationship to stresses.

Quantifying the ways in which local particle rearrangements contribute to macroscopic plasticity is one of the fundamental pursuits of granular mechanics and soft matter physics. Here we examine local rearrangements that occur naturally during the deformation of three samples of 3D granular materials subjected to distinct boundary conditions by employing in situ x-ray measurements of particle-resolved structure and stress. We focus on five distinct rearrangement measures, their statistics, interrelationships, contributions to macroscopic deformation, repeatability, and dependence on local structure and stress. Our most significant findings are that local rearrangements (1) are correlated on a scale of three to four particle diameters, (2) exhibit volumetric strain-shear strain and nonaffine displacement-rotation coupling, (3) exhibit correlations that suggest either rearrangement repeatability or that rearrangements span multiple steps of incremental sample strain, and (4) show little dependence on local stress but correlate with quantities describing local structure, such as porosity. Our results are presented in the context of relevant plasticity theories and are consistent with recent findings suggesting that local structure may play at least as important of a role as local stress in determining the nature of local rearrangements.

Characterisation of Single-Phase Fluid-Flow Heterogeneity Due to Localised Deformation in a Porous Rock Using Rapid Neutron Tomography.

The behaviour of subsurface-reservoir porous rocks is a central topic in the resource engineering industry and has relevant applications in hydrocarbon, water production, and CO2 sequestration. One of the key open issues is the effect of deformation on the hydraulic properties of the host rock and, specifically, in saturated environments. This paper presents a novel full-field data set describing the hydro-mechanical properties of porous geomaterials through in situ neutron and X-ray tomography. The use of high-performance neutron imaging facilities such as CONRAD-2 (Helmholtz-Zentrum Berlin) allows the tracking of the fluid front in saturated samples, making use of the differential neutron contrast between "normal" water and heavy water. To quantify the local hydro-mechanical coupling, we applied a number of existing image analysis algorithms and developed an array of bespoke methods to track the water front and calculate the 3D speed maps. The experimental campaign performed revealed that the pressure-driven flow speed decreases, in saturated samples, in the presence of pre-existing low porosity heterogeneities and compactant shear-bands. Furthermore, the observed complex mechanical behaviour of the samples and the associated fluid flow highlight the necessity for 3D imaging and analysis.

A Continuity Flow Based Tomographic Reconstruction Algorithm for 4D Multi-Beam High Temporal-Low Angular Sampling.

A mathematical framework and accompanying numerical algorithm exploiting the continuity equation for 4D reconstruction of spatiotemporal attenuation fields from multi-angle full-field transmission measurements is presented. The algorithm is geared towards rotation-free dynamic multi-beam X-ray tomography measurements, for which angular information is sparse but the temporal information is rich. 3D attenuation maps are recovered by propagating an initial discretized density volume in time according to the advection equations using the Finite Volumes method with a total variation diminishing monotonic upstream-centered scheme (TVDMUSCL). The benefits and limitations of the algorithm are explored using dynamic granular system phantoms modelled via discrete elements and projected by an analytical ray model independent from the numerical ray model used in the reconstruction scheme. Three phantom scenarios of increasing complexity are presented and it is found that projections from only a few (unknowns:equations > 10) angles can be sufficient for characterisation of the 3D attenuation field evolution in time. It is shown that the artificial velocity field produced by the algorithm sub-iteration, which is used to propagate the attenuation field, can to some extent approximate the true kinematics of the system. Furthermore, it is found that the selection of a temporal interpolation scheme for projection data can have a significant impact on error build up in the reconstructed attenuation field.

Dual modality neutron and x-ray tomography for enhanced image analysis of the bone-metal interface.

The bone tissue formed at the contact interface with metallic implants, particularly its 3D microstructure, plays a pivotal role for the structural integrity of implant fixation. X-ray tomography is the classical imaging technique used for accessing microstructural information from bone tissue. However, neutron tomography has shown promise for visualising the immediate bone-metal implant interface, something which is highly challenging with x-rays due to large differences in attenuation between metal and biological tissue causing image artefacts. To highlight and explore the complementary nature of neutron and x-ray tomography, proximal rat tibiae with titanium-based implants were imaged with both modalities. The two techniques were compared in terms of visualisation of different material phases and by comparing the properties of the individual images, such as the contrast-to-noise ratio. After superimposing the images using a dedicated image registration algorithm, the complementarity was further investigated via analysis of the dual modality histogram, joining the neutron and x-ray data. From these joint histograms, peaks with well-defined grey value intervals corresponding to the different material phases observed in the specimens were identified and compared. The results highlight differences in how neutrons and x-rays interact with biological tissues and metallic implants, as well as the benefits of combining both modalities. Future refinement of the joint histogram analysis could improve the segmentation of structures and tissues, and yield novel information about specimen-specific properties such as moisture content.

Lupin Protein Isolate Structure Diversity in Frozen-Cast Foams: Effects of Transglutaminases and Edible Fats.

This study addresses an innovative approach to generate aerated foods with appealing texture through the utilization of lupin protein isolate (LPI) in combination with edible fats. We show the impact of transglutaminases (TGs; SB6 and commercial), glycerol (Gly), soy lecithin (Lec) and linoleic acid (LA) on the micro- and nanostructure of health promoting solid foods created from LPI and fats blends. 3-D tomographic images of LPI with TG revealed that SB6 contributed to an exceptional bubble spatial organization. The inclusion of Gly and Lec decreased protein polymerization and also induced the formation of a porous layered material. LA promoted protein polymerization and formation of homogeneous thick layers in the LPI matrix. Thus, the LPI is a promising protein resource which when in blend with additives is able to create diverse food structures. Much focus has been placed on the great foamability of LPI and here we show the resulting microstructure of LPI foams, and how these were improved with addition of TGs. New food applications for LPI can arise with the addition of food grade dispersant Lec and essential fatty-acid LA, by improved puffiness, and their contributing as replacer of chemical leavening additives in gluten-free products.

3D-printed monolithic biofilters based on a polylactic acid (PLA) - hydroxyapatite (HAp) composite for heavy metal removal from an aqueous medium.

High flux, monolithic water purification filters based on polylactic acid (PLA) functionalised with fish scale extracted hydroxyapatite (HAp) were prepared by solvent-assisted blending and thermally induced phase separation (TIPS), followed by twin-screw extrusion into filaments and processed via three-dimensional (3D) printing. The printed filters with consistent pore geometry and channel interconnectivity as well as homogenous distribution of HAp in the PLA matrix showed adsorption capabilities towards heavy metals i.e. cadmium (Cd) and lead (Pb) with maximum adsorption capacity of 112.1 mg gHAp -1 and 360.5 mg gHAp -1 for the metal salt of Pb and Cd, respectively. The adsorption was found to be driven by a combination of ion exchange, dissolution and precipitation on HAp and surface complexation.

Sub-trabecular strain evolution in human trabecular bone.

To comprehend the most detrimental characteristics behind bone fractures, it is key to understand the material and tissue level strain limits and their relation to failure sites. The aim of this study was to investigate the three-dimensional strain distribution and its evolution during loading at the sub-trabecular level in trabecular bone tissue. Human cadaver trabecular bone samples were compressed in situ until failure, while imaging with high-resolution synchrotron radiation X-ray tomography. Digital volume correlation was used to determine the strains inside the trabeculae. Regions without emerging damage were compared to those about to crack. Local strains in close vicinity of developing cracks were higher than previously reported for a whole trabecular structure and similar to those reported for single isolated trabeculae. Early literature on bone fracture strain thresholds at the tissue level seem to underestimate the maximum strain magnitudes in trabecular bone. Furthermore, we found lower strain levels and a reduced ability to capture detailed crack-paths with increased image voxel size. This highlights the dependence between the observed strain levels and the voxel size and that high-resolution is needed to investigate behavior of individual trabeculae. Furthermore, low trabecular thickness appears to be one predictor of developing cracks. In summary, this study investigated the local strains in whole trabecular structure at sub-trabecular resolution in human bone and confirmed the high strain magnitudes reported for single trabeculae under loading and, importantly extends its translation to the whole trabecular structure.

Bone Damage Evolution Around Integrated Metal Screws Using X-Ray Tomography - in situ Pullout and Digital Volume Correlation.

Better understanding of the local deformation of the bone network around metallic implants subjected to loading is of importance to assess the mechanical resistance of the bone-implant interface and limit implant failure. In this study, four titanium screws were osseointegrated into rat tibiae for 4 weeks and screw pullout was conducted in situ under x-ray microtomography, recording macroscopic mechanical behavior and full tomographies at multiple load steps before failure. Images were analyzed using Digital Volume Correlation (DVC) to access internal displacement and deformation fields during loading. A repeatable failure pattern was observed, where a ∼300-500 µm-thick envelope of bone detached from the trabecular structure. Fracture initiated close to the screw tip and propagated along the implant surface, at a distance of around 500 µm. Thus, the fracture pattern appeared to be influenced by the microstructure of the bone formed closely around the threads, which confirmed that the model is relevant for evaluating the effect of pharmacological treatments affecting local bone formation. Moreover, cracks at the tibial plateau were identified by DVC analysis of the tomographic images acquired during loading. Moderate strains were first distributed in the trabecular bone, which localized into higher strains regions with subsequent loading, revealing crack-formation not evident in the tomographic images. The in situ loading methodology followed by DVC is shown to be a powerful tool to study internal deformation and fracture behavior of the newly formed bone close to an implant when subjected to loading. A better understanding of the interface failure may help improve the outcome of surgical implants.

Reconstructing intragranular strain fields in polycrystalline materials from scanning 3DXRD data.

Two methods for reconstructing intragranular strain fields are developed for scanning three-dimensional X-ray diffraction (3DXRD). The methods are compared with a third approach where voxels are reconstructed independently of their neighbours [Hayashi, Setoyama & Seno (2017). Mater. Sci. Forum, 905, 157-164]. The 3D strain field of a tin grain, located within a sample of approximately 70 grains, is analysed and compared across reconstruction methods. Implicit assumptions of sub-problem independence, made in the independent voxel reconstruction method, are demonstrated to introduce bias and reduce reconstruction accuracy. It is verified that the two proposed methods remedy these problems by taking the spatial properties of the inverse problem into account. Improvements in reconstruction quality achieved by the two proposed methods are further supported by reconstructions using synthetic diffraction data.

Exploring the visual world of fossilized and modern fungus gnat eyes (Diptera: Keroplatidae) with X-ray microtomography.

Animal eyes typically possess specialized regions for guiding different behavioural tasks within their specific visual habitat. These specializations, and evolutionary changes to them, can be crucial for understanding an animal's ecology. Here, we explore how the visual systems of some of the smallest flying insects, fungus gnats, have adapted to different types of forest habitat over time (approx. 30 Myr to today). Unravelling how behavioural, environmental and phylogenetic factors influence the evolution of visual specializations is difficult, however, because standard quantitative techniques often require fresh tissue and/or provide data in eye-centric coordinates that prevent reliable comparisons between species with different eye morphologies. Here, we quantify the visual world of three gnats from different time periods and habitats using X-ray microtomography to create high-resolution three-dimensional models of the compound eyes of specimens in different preservation states-fossilized in amber, dried or stored in ethanol. We present a method for analysing the geometric details of individual corneal facets and for estimating and comparing the sensitivity, spatial resolution and field of view of species across geographical space and evolutionary time. Our results indicate that, despite their miniature size, fungus gnats do have variations in visual properties across their eyes. We also find some indication that these visual specializations vary across species and may represent adaptations to their different forest habitats. Overall, the findings demonstrate how such investigations can be used to study the evolution of visual specializations-and sensory ecology in general-across a range of insect taxa from different geographical locations and across time.

Fossil insect eyes shed light on trilobite optics and the arthropod pigment screen.

Fossilized eyes permit inferences of the visual capacity of extinct arthropods1-3. However, structural and/or chemical modifications as a result of taphonomic and diagenetic processes can alter the original features, thereby necessitating comparisons with modern species. Here we report the detailed molecular composition and microanatomy of the eyes of 54-million-year-old crane-flies, which together provide a proxy for the interpretation of optical systems in some other ancient arthropods. These well-preserved visual organs comprise calcified corneal lenses that are separated by intervening spaces containing eumelanin pigment. We also show that eumelanin is present in the facet walls of living crane-flies, in which it forms the outermost ommatidial pigment shield in compound eyes incorporating a chitinous cornea. To our knowledge, this is the first record of melanic screening pigments in arthropods, and reveals a fossilization mode in insect eyes that involves a decay-resistant biochrome coupled with early diagenetic mineralization of the ommatidial lenses. The demonstrable secondary calcification of lens cuticle that was initially chitinous has implications for the proposed calcitic corneas of trilobites, which we posit are artefacts of preservation rather than a product of in vivo biomineralization4-7. Although trilobite eyes might have been partly mineralized for mechanical strength, a (more likely) organic composition would have enhanced function via gradient-index optics and increased control of lens shape.

Scanning 3DXRD Measurement of Grain Growth, Stress, and Formation of Cu6Sn5 around a Tin Whisker during Heat Treatment.

The 3D microstructure around a tin whisker, and its evolution during heat treatment were studied using scanning 3DXRD. The shape of each grain in the sample was reconstructed using a filtered-back-projection algorithm. The local lattice parameters and grain orientations could then be refined, using forward modelling of the diffraction data, with a spatial resolution of 250 n m . It was found that the tin coating had a texture where grains were oriented such that their c-axes were predominantly parallel to the sample surface. Grains with other orientations were consumed by grain growth during the heat treatment. Most of the grain boundaries were found to have misorientations larger than 15 ∘ , and many coincidence site lattice (CSL) or other types of low-energy grain boundaries were identified. None of the grains with CSL grain boundaries were consumed by grain growth. During the heat treatment, growth of preexisting Cu6Sn5 occurred; these grains were indexed as a hexagonal η phase, which is usually documented to be stable only at temperatures exceeding 186 ∘ C . This indicates that the η phase can exist in a metastable state for long periods. The tin coating was found to be under compressive hydrostatic stress, with a negative gradient in hydrostatic stress extending outwards from the root of the whisker. Negative stress gradients are generally believed to play an essential role in providing the driving force for diffusion of material to the whisker root.

Linking multiscale deformation to microstructure in cortical bone using in situ loading, digital image correlation and synchrotron X-ray scattering.

The incidence of fragility fractures is expected to increase in the near future due to an aging population. Therefore, improved tools for fracture prediction are required to treat and prevent these injuries efficiently. For such tools to succeed, a better understanding of the deformation mechanisms in bone over different length scales is needed. In this study, an experimental setup including mechanical tensile testing in combination with digital image correlation (DIC) and small/wide angle X-ray scattering (SAXS/WAXS) was used to study deformation at multiple length scales in bovine cortical bone. Furthermore, micro-CT imaging provided detailed information about tissue microstructure. The combination of these techniques enabled measurements of local deformations at the tissue- and nanoscales. The orientation of the microstructure relative to the tensile loading was found to influence the strain magnitude on all length scales. Strains in the collagen fibers were 2-3 times as high as the strains found in the mineral crystals for samples with microstructure oriented parallel to the loading. The local tissue strain at fracture was found to be around 0.5%, independent of tissue orientation. However, the maximum force and the irregularity of the crack path were higher when the load was applied parallel to the tissue orientation. This study clearly shows the potential of combining these different experimental techniques concurrently with mechanical testing to gain a better understanding of bone damage and fracture over multiple length scales in cortical bone. STATEMENT OF SIGNIFICANCE: To understand the pathophysiology of bone, it is important to improve our knowledge about the deformation and fracture mechanisms in bone. In this study, we combine several recently available experimental techniques with mechanical loading to investigate the deformation mechanisms in compact bone tissue on several length scales simultaneously. The experimental setup included mechanical tensile testing in combination with digital image correlation, microCT imaging, and small/wide angle X-ray scattering. The combination of techniques enabled measurements of local deformations at the tissue- and nanoscales. The study clearly shows the potential of combining different experimental techniques concurrently with mechanical testing to gain a better understanding of structure-property-function relationships in bone tissue.

'Phoenix polymers': fire induced nanohardness in fibril-forming aromatic cyanate esters.

For the first time we present nanoindentation analysis of charred, cured aromatic cyanate esters, which exhibit outstanding mechanical properties when analysed under applied loads of 0.1-300 mN. Following charring (900 °C for 10 minutes to achieve graphitised structures), the samples display a remarkable combination of a modulus of elasticity of around 25 GPa and nanohardness of 300 kgf mm-2, making them some 30-40% stiffer than bone and practically as hard as tooth enamel. At the same time we find that under the same conditions the chars are highly resilient, displaying complete elastic recovery with very little plastic deformation. When cured in the presence of copper(ii) acetylacetonate (200 ppm) in dodecylphenol (1% w/v active copper suspension) to form a polycyanurate, compound (2) forms a dense, consolidated structure compared with compound (1) under the same conditions. At high magnification, the presence of a nanoscale, fibrillar structure is observed, accounting for the high resilience.

Investigating the Mechanical Characteristics of Bone-Metal Implant Interface Using in situ Synchrotron Tomographic Imaging.

Long-term stability of endosseous implants depends on successful bone formation, ingrowth and adaptation to the implant. Specifically, it will define the mechanical properties of the newly formed bone-implant interface. 3D imaging during mechanical loading tests (in situ loading) can improve the understanding of the local processes leading to bone damage and failure. In this study, titanium screws were implanted into rat tibiae and were allowed to integrate for 4 weeks with or without the addition of the growth factor Bone Morphogenetic Protein and the bisphosphonate Zoledronic Acid. Samples were subjected to in situ pullout using high-resolution synchrotron x-ray tomography at the Tomcat beamline (SLS, PSI, Switzerland) at 30 keV with 25 ms exposure time, resulting in a total acquisition time of 45 s per scan, with a 3.6 µm isotropic voxel size. Using a custom-made loading device positioned inside the beamline, screws were pulled out with 0.05 mm increment, acquiring multiple scans until rupture of the sample. The in situ loading protocol was adapted to ensure short imaging time, which enabled multiple samples to be tested with short loading steps, while keeping the total testing time low and reducing dose deposition. Higher trabecular bone content was quantified in the surrounding of the screw in the treated groups, which correlated with increased mechanical strength and stiffness. Differences in screw implantation, such as contact between threads and cortex as well as minor tilt of the screw were also correlated to the mechanical parameters. In situ loading enabled the investigation of crack propagation during the pullout, highlighting the mechanical behavior of the interface. Three typical crack types were observed: (1) rupture at the interface of trabecular and cortical bone tissues, close to the screw, (2) large crack inside the cortex connected to the implant, and (3) first failure away from the screw with cracks propagating toward the screw-bone interface. Mechanical properties of in vivo integrated bone-metal screws rely on a combination of multiple parameters that are difficult to identify and separate one from the other.

Time-of-Flight Three Dimensional Neutron Diffraction in Transmission Mode for Mapping Crystal Grain Structures.

The physical properties of polycrystalline materials depend on their microstructure, which is the nano- to centimeter scale arrangement of phases and defects in their interior. Such microstructure depends on the shape, crystallographic phase and orientation, and interfacing of the grains constituting the material. This article presents a new non-destructive 3D technique to study centimeter-sized bulk samples with a spatial resolution of hundred micrometers: time-of-flight three-dimensional neutron diffraction (ToF 3DND). Compared to existing analogous X-ray diffraction techniques, ToF 3DND enables studies of samples that can be both larger in size and made of heavier elements. Moreover, ToF 3DND facilitates the use of complicated sample environments. The basic ToF 3DND setup, utilizing an imaging detector with high spatial and temporal resolution, can easily be implemented at a time-of-flight neutron beamline. The technique was developed and tested with data collected at the Materials and Life Science Experimental Facility of the Japan Proton Accelerator Complex (J-PARC) for an iron sample. We successfully reconstructed the shape of 108 grains and developed an indexing procedure. The reconstruction algorithms have been validated by reconstructing two stacked Co-Ni-Ga single crystals, and by comparison with a grain map obtained by post-mortem electron backscatter diffraction (EBSD).