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A combination of characterization techniques has been used to provide new understanding of the complex crystallization behavior of as-sprayed amorphous Yb2Si2O7-based air-plasma-sprayed environmental barrier coatings (EBCs). During crystallization heat-treatment, initially a mixture of metastable α-Yb2Si2O7 and X1-Yb2SiO5 phases form, along with stable β-Yb2Si2O7 and X2-Yb2SiO5 phases. Eventually the metastable phases transform to the stable β-Yb2Si2O7 (major) and X2-Yb2SiO5 (minor) phases. The significant volume expansion associated with these transformations partially contributes towards the anomalous expansion measured in these EBCs after crystallization, but it does not account for all the measured expansion. In this context, in similar EBCs, it is also observed that the porosity increases upon crystallization heat-treatment, primarily in the form of thin, interconnected pores, which also contributes to the measured anomalous expansion. Based on this understanding, guidelines are provided for ‘near-net-shape’ crystallization of phase-pure, dense β-Yb2Si2O7 EBCs that are free of vertical cracks.

Single crystals of rhombohedral KBiS2 were synthesized for the first time, and the structure, growth habit and properties of this layered semiconductor are presented. The single crystals form from a reactive K2S5 salt flux and are still embedded in the residual flux, without removal from the reaction vessel throughout the whole study. Laboratory diffraction contrast tomography (LabDCT) is used to identify the crystalline phase, orientation, and microstructure of crystals. Meanwhile, powder and single crystal X-ray diffraction were performed to determine detailed crystallographic information. Morphology of the crystalline assemblies observed by absorption contrast tomography reveals screw-dislocation-driven growth to be the dominant mechanism. First-principles electronic structure simulations predict rhombohedral KBiS2 to be a semiconductor with an indirect band gap, which was confirmed by experiment. This study demonstrates how non-destructive tomography imaging and 3D crystallography methods can lead to advances in discovering new materials and studying crystal growth mechanisms.

Volume fracturing in horizontal wells represents a principal technology in the effective economic development of unconventional shale oil and gas reservoirs. However, the number of intervals that were effectively fractured by this technology only account for 20%–50% of the total designed sections. Fracture development characteristics and the factors controlling artificial fracture growth in organic-rich shale require detailed evaluation; this cannot be accomplished using microseismic monitoring technology or well-log interpretation. In this paper, formation processes of micro- and nano-scale fractures in the organic-rich shales of the Lucaogou Formation, Jimusaer Sag, Junggar Basin, northwestern China, were presented. The study focused on the application of in situ, nano-scale CT imaging technology, in combination with rock mechanics analysis. Results allowed the visualization of fracture growth in the shale reservoirs, and revealed the influence of organic matter, mineral composition, and pore structure on the formation and distribution of artificial fractures. A three-dimensional dynamic growth model of micro- and nano-scale fractures in organic-rich shale was established. Data revealed that the Lucaogou Formation shale contained dolomite and illite intragranular pores, with a low abundance of organic pores; pore size ranged between 200 nm and 2 μm. Micro- and nano-size fractures were observed. The development of artificial fractures was positively correlated with the loading stress. The initiation stress of new generated fractures was 475 mN, which could break up dolomite, albite, K-feldspar, and the original pore system as well. The original pore system was generally conducive to fracture extension and expansion. As loading stress increased from 50 mN to 515 mN, the sample extension increased from 2 μm to 14 μm, and artificial fracture width increased from 0.3 μm to 10 μm. The total porosity increased from 5.45% to 8.35%, and volume growth rate reached 53.2%. These findings provide valuable insights into the study of fracture growth in organic-rich shales, and have implications for the design of hydro-fracturing in organic-rich shales.

Laboratory diffraction contrast tomography (LabDCT) enables the user to reconstruct three-dimensional (3D) grain maps of polycrystalline materials. For each grain, the size, orientation, and 3D morphology including the number of faces can be derived. Since the technique is non-destructive, LabDCT opens up new possibilities for studies of microstructural evolution at the level of individual grains. The LabDCT setup is integrated on a commercial X-ray microscope, enabling correlation of the resulting grain map with complimentary information on, e.g., cracks, porosities, and inclusions. Here, the LabDCT principle is introduced, and recent materials science applications are presented. The first example on liquid metal embrittlement highlights the correlation of grain boundary properties and complimentary absorption information on grain boundary wetting. It is shown that the grain boundary energy determines whether wetting occurs or not. The second example is on grain growth. The grain statistics in this study, more than 1200 grains at two different time steps, were large enough to capture rare events such as abnormal grain growth and the annihilation of a grain with only three faces.

In situ studies using X-ray tomography have gained immense popularity in the recent past owing to their non-destructive nature and ability to capture the microstructure of a wide range of materials in 3D. In this work, we have conducted in situ micropillar compression and studied damage evolution in Al/SiC nanolaminates using a laboratory-based nanoscale X-ray microscope. Nanoscale defects present in the microstructure were characterized in 3D. The effect of these nanopores on damage initiation was quantified and is discussed. Additionally, the effect of Ga+ ion milling on micropillar fabrication was characterized by performing a comparative experiment on pillars fabricated using Ga+ and Ne+ ion source based focused ion beams.

A fundamental understanding of the behaviour of polycrystalline materials, including pharmaceuticals, is vital for control of their physicochemical and crystalline properties, which in turn has the potential to improve drug product development for example. In this work, attenuation X-ray Computed Tomography (CT) and Diffraction Contrast Tomography (DCT) are combined with molecular modelling to understand the powder packing behaviour and crystal interactions of the organic cubic compound hexamine (hexamethylenetetramine). It is the first application of DCT to polycrystalline organic materials. The crystal morphology is predicted through synthonic modelling, with fully 3D-resolved confirmation of the crystallography of the external {110} facets, edges and corner directions through DCT. Analysis of the powder-bed reveals agglomerate structures and orientational texture, with its chemical origins energetically predicted to be face-to-face in accordance with the experimental data. Finally, measurements of crystal & crystallite interactions provide evidence for different mechanisms of powder bed agglomeration.

Excessive skeletal deformations and brittle fractures in the vast majority of patients suffering from osteogenesis imperfecta (OI) are a result of substantially reduced bone quality. Because the mechanical competence of bone is dependent on the tissue characteristics at small length scales, it is of crucial importance to assess how OI manifests at the micro- and nanoscale of bone. In this context, the Chihuahua (Chi/+) zebrafish, carrying a heterozygous glycine substitution in the α1 chain of collagen type I, has recently been proposed as a suitable animal model of classical dominant OI, showing skeletal deformities, altered mineralization patterns, and a smaller body size. This study assessed the bone quality properties of Chi/+ at multiple length scales using micro-computed tomography (micro-CT), histomorphometry, quantitative back-scattered electron imaging, Fourier-transform infrared spectroscopy, nanoindentation, and X-ray microscopy. At the skeletal level, the Chi/+ displays smaller body size, deformities, and fracture calli in the ribs. Morphological changes at the whole bone level showed that the vertebrae in Chi/+ had a smaller size, smaller thickness, and distorted shape. At the tissue level, Chi/+ displayed a higher degree of mineralization, lower collagen maturity, lower mineral maturity, altered osteoblast morphology, and lower osteocyte lacunar density compared to wild-type zebrafish. The alterations in the cellular, compositional, and structural properties of Chi/+ bones bear an explanation for the impaired local mechanical properties, which promote an increase in overall bone fragility in Chi/+. The quantitative assessment of bone quality in Chi/+ thus further validates this mutant as an important model reflecting osseous characteristics associated with human classical dominant OI. © 2018 American Society for Bone and Mineral Research.

Most technologically-relevant materials exhibit a microstructural heterogeneity over multiple length scales, and it is this heterogeneity that ultimately determines their performance. For example, the efficiency of polycrystalline silicon (poly-Si) photovoltaic cells is critically dependent on the nature of the grain boundaries and foreign metal impurities in the bulk. Here, we probe the characteristics and distributions of these defects in three dimensions by using a novel, integrated, and non-destructive imaging platform. In particular, recent advances in laboratory-based diffraction contrast tomography (LabDCT) enable us to measure grain centroid, volume, orientation, and shape. From this crystallographic information, we extract the five-parameter grain boundary distributions in poly-Si. By using a combination of LabDCT, attenuation-based tomography, and electron microscopy, we determine that the location of the impurity particles is non-random in the bulk and strongly dependent on grain boundary character. The correlative analysis not only demonstrates the degree of interaction between foreign metal impurities and structural defects in poly-Si, but also highlights the viability of burgeoning tomographic methods such as LabDCT. It is anticipated that our integrated approach can be extended to other complex microstructures with minimal sample-specific tuning.

3D printing is a process of hierarchically fabricating three-dimensional microstructures by successively adding materials in a bottom-up manner. The technology has been rapidly advancing, especially in the manufacturing of high-strength, lightweight industrial composite materials. Thus far, many studies have focused on the spontaneous alignment of short reinforcing fibers that are subject to adjustment during the 3D-printing process, along with an inevitable void formation arising due to an intrinsic nature of the additive process. However, systematic examination of the 3D-printed anisotropic microstructures, related with a markedly high degree of fiber alignment and formation of voids in the matrix, has not been sufficiently conducted to analyze its effect on the anisotropic mechanical behaviors of fiber-reinforced composites. Here, we sought to examine in detail the internal morphology of fibers and voids in 3D-printed composites by 3D X-ray microscopy to explore their anisotropic architecture. The position, length, and alignment of fibers and voids were identified, visualized, and quantitatively characterized with a help of computational tomography (CT). Furthermore, the anisotropy approximation of the 3D-printed composites, precisely predicted through CT-assisted simulation, was derived based on the quantitative data obtained from the 3D reconstruction image. These measurements were effective in exploring the process-induced alignment nature of fibers and voids in the local region layers on the microscopic scale, and the corresponding microstructure resulted in a change in the elastic modulus of the composites with the printing direction. The comparative results showed that the experimental results were well supported by the simulation-based estimations, but did not exactly match the rule-of-mixture of the composites in terms of interfacial nature due to the distinctive microstructure with the fiber-to-matrix interface as well as the filament-to-filament interface.

All levels of the unique hierarchical structure of bone, consisting of collagen and hydroxyapatite crystals at the nanoscale to osteon/lamellae structures at the microscale, contribute to its characteristic toughness and material properties. Elements of bone's density and size contribute to bone quantity (or bone mass), whereas elements of bone's material composition, material properties, internal structure, and organization describe bone quality. Bone quantity and quality can be degraded by factors such as aging, disease, treatments, and irradiation, compromising its ability to resist fracture and sustain loading. Accessing the morphology and architecture of bone at the microscale to quantify microstructural features and assess the degree of mineralization and path of crack propagation in bone provides crucial information on how these factors are influencing bone quantity and quality. Synchrotron radiation micro-computed tomography (SRμCT) was first used to assess bone structure at the end of the 1990's. One of the main advantages of the technique is that it enables accurate three-dimensional (3D), non-destructive quantification of structure while traditional histomorphometry on histological sections is inherantly destructive to the sample and two-dimensional (2D). Additionally, SRμCT uses monochromatic, high-flux X-ray beams to provide high-resolution and high-contrast imaging of bone samples. This allows the quantification of small microstructural features (e.g. osteocyte lacunae, canals, trabeculae, microcracks) and direct gray value compositional mapping (e.g. mineral quantification, cement lines) with greater speed and fidelity than lab-based micro-computed tomography. In this article, we review how SRμCT has been applied to bone research to elucidate the mechanisms by which bone aging, disease, and other factors affect bone fragility and resistance to fracture.

A method for the solidification of metallic alloys involving spiral self-organization is presented as a new strategy for producing large-area chiral patterns with emergent structural and optical properties, with attention to the underlying mechanism and dynamics. This study reports the discovery of a new growth mode for metastable, two-phase spiral patterns from a liquid metal. Crystallization proceeds via a non-classical, two-step pathway consisting of the initial formation of a polytetrahedral seed crystal, followed by ordering of two solid phases that nucleate heterogeneously on the seed and grow in a strongly coupled fashion. Crystallographic defects within the seed provide a template for spiral self-organization. These observations demonstrate the ubiquity of defect-mediated growth in multi-phase materials and establish a pathway toward bottom-up synthesis of chiral materials with an inter-phase spacing comparable to the wavelength of infrared light. Given that liquids often possess polytetrahedral short-range order, our results are applicable to many systems undergoing multi-step crystallization.

Research across science domains is increasingly reliant on image-centric data. Software tools are in high demand to uncover relevant, but hidden, information in digital images, such as those coming from faster next generation high-throughput imaging platforms. The challenge is to analyze the data torrent generated by the advanced instruments efficiently, and provide insights such as measurements for decision-making. In this paper, we overview work performed by an interdisciplinary team of computational and materials scientists, aimed at designing software applications and coordinating research efforts connecting (1) emerging algorithms for dealing with large and complex datasets; (2) data analysis methods with emphasis in pattern recognition and machine learning; and (3) advances in evolving computer architectures. Engineering tools around these efforts accelerate the analyses of image-based recordings, improve reusability and reproducibility, scale scientific procedures by reducing time between experiments, increase efficiency, and open opportunities for more users of the imaging facilities. This paper describes our algorithms and software tools, showing results across image scales, demonstrating how our framework plays a role in improving image understanding for quality control of existent materials and discovery of new compounds.

Whether it be the mechanical response of biomaterials or the crack propagation pathways within metal alloys, observing how damage occurs (both spatially and temporally) is critical to understanding materials behavior. Here, nanoscale transmission X-ray microscopy (TXRM) is used to follow the initiation and propagation of damage during quasi-static mechanical testing of natural, crystalline, and metallic materials. The coupling of a novel load stage and TXRM for in situ mechanical testing enables both radiographic (2D) and tomographic (3D) characterization. With an imaging resolution down to 50 nm during uniaxial nanoindentation, compression, or tension, TXRM is ideally suited for the characterization of materials degradation. Several applications are demonstrated including nanoindentation of dentin, compression of a single crystal of high explosive, and tensile testing of both beetle cuticle and Al-Cu alloy. These experiments highlight the capability of the new experimental fixture to provide enhanced insight on material performance through four dimensional (3D + time) observation and analysis.

The ability to accurately map crystal grain morphology and grain boundaries in polycrystalline materials, non-destructively and in three-dimensions is required for detailed investigations into many aspects of polycrystalline deformation, as well as many other properties. Previously, the laboratory-based X-ray diffraction contrast tomography technique (LabDCT) has been shown to be capable of reconstructing crystallographic orientations and grain centres in 3D. Here we demonstrate the extension of the method to the reconstruction of the individual 3D grain shapes. Firstly, the grain boundaries are mapped by DCT in a beta‑titanium alloy (Ti-β21S) sample and validated by independent measurements of the grain shapes obtained from phase contrast tomography. The independent validation measurements show that the boundaries can be located with a mean accuracy of 4.4 μm. Secondly, the grain locations and orientations in a copper powder sample sintered at 1050 °C are tracked over time in a time-lapse manner by LabDCT and then the final state compared and validated against destructive serial sectioning EBSD (3D-EBSD) post-mortem. In this case we are able to follow the recrystallisation and competitive grain growth over time, by visualising the migration of selected grain boundaries. In particular the shrinkage and dissolution of grains in the immediate vicinity of a fast-growing grain are observed and quantified in the light of changes in misorientation relationships with the growing grain. More generally, LabDCT can be used to characterise, track or establish realistic 3D image-based models of polycrystalline microstructures across a range of crystal structures.

The characteristics of fracture propagation in heterogeneous tight sandstones are critical to volumetric fracturing, which is the key to unlocking unconventional resources in tight sandstones. Quantification of the influence of pre-existing pore systems and particle arrangements on the propagation of fractures is challenging due to inadequate imaging of the internal void systems in tight sandstones from three-dimensional (3D) aspect. In this study, the 3D geometry of tight sandstones from the Chang 7 member in the Ordos Basin is continuously imaged under different loading stresses, and the voxel resolution of the X-ray computed tomography is 2.5 μm. The data set captured in this process shows the changes in the samples at the microstructural level as they approach fracturing. The data are stored as a time series of 3D images. The results demonstrate that: (i) fractures propagate progressively and gradually link with pre-existing pores, resulting in macroscopic fractures with a maximum width of 250 μm, while newly generated fractures could break up particles and may not follow the line of pre-existing fractures; and (ii) three stages were identified in the failure process of tight sandstones, with new fractures running at an angle of about 30° to the general direction of the stress of compression. The total volumes of both the sample and pore-fractures, and the damage index, which were extracted from the 3D images, all increased when approaching fracturing. The final volume of pore-fracture systems could be 11 times that of the initial pore volume. All of these observations provide valuable insights and design guidelines for hydraulic fracturing in unconventional tight sandstones, and a quantified model of the dynamics and the morphology of fracture propagation with increasing stress approaching failure, which may shed light on dynamic critical transitions in the Earth's crust.

A novel reconstruction method to retrieve grain structure from laboratory diffraction contrast tomography is presented and evaluated., A method for reconstructing the three-dimensional grain structure from data collected with a recently introduced laboratory-based X-ray diffraction contrast tomography system is presented. Diffraction contrast patterns are recorded in Laue-focusing geometry. The diffraction geometry exposes shape information within recorded diffraction spots. In order to yield the three-dimensional crystallographic microstructure, diffraction spots are extracted and fed into a reconstruction scheme. The scheme successively traverses and refines solution space until a reasonable reconstruction is reached. This unique reconstruction approach produces results efficiently and fast for well suited samples.

Exercise promotes gain in bone mass through adaptive responses of the vertebrate skeleton. This mechanism counteracts age- and disease-related skeletal degradation, but remains to be fully understood. In life sciences, zebrafish emerged as a vertebrate model that can provide new insights into the complex mechanisms governing bone quality. To test the hypothesis that musculoskeletal exercise induces bone adaptation in adult zebrafish and to characterize bone reorganization, animals were subjected to increased physical exercise for four weeks in a swim tunnel experiment. Cellular, structural and compositional changes of loaded vertebrae were quantified using integrated high-resolution analyses. Exercise triggered rapid bone adaptation with substantial increases in bone-forming osteoblasts, bone volume and mineralization. Clearly, modeling processes in zebrafish bone resemble processes in human bone. This study highlights how exercise experiments in adult zebrafish foster in-depth insight into aging-related bone diseases and can thus catalyze the search for appropriate prevention and new treatment options.

article i nfo Bisphosphonates are widely used to treat osteoporosis, but have been associated with atypical femoral fractures (AFFs) in the long term, which raises a critical health problem for the aging population. Several clinical studies havesuggested that theoccurrence of AFFs may berelated tothe bisphosphonate-induced changes of bone turn- over, but large discrepancies in the results of these studies indicate that the salient mechanisms responsible for any loss in fracture resistance are still unclear. Here the role of bisphosphonates is examined in terms of the po- tential deterioration in fracture resistance resulting from both intrinsic (plasticity) and extrinsic (shielding) toughening mechanisms, which operate over a wide range of length-scales. Specifically, we compare the me- chanical properties of two groups of humeri from healthy beagles, one control group comprising eight females (oral doses of saline vehicle, 1 mL/kg/day, 3 years) and one treated group comprising nine females (oral doses of alendronate used to treat osteoporosis, 0.2 mg/kg/day, 3 years). Our data demonstrate treatment-specifi cr e- organization of bone tissue identified at multiple length-scales mainly through advanced synchrotron x-ray ex- periments. We confirm that bisphosphonate treatments can increase non-enzymatic collagen cross-linking at molecular scales, which critically restricts plasticity associated with fibrillar sliding, and hence intrinsic toughen- ing, at nanoscales. We also observe changes in the intracortical architecture of treated bone at microscales, with partial fillingof the Haversiancanalsandreductionof osteon number.We hypothesize thatthereducedplasticity associated with BP treatmentsmay induce an increaseinmicrocrack accumulation and growth undercyclic daily loadings, and potentially increase the susceptibility of cortical bone to atypical (fatigue-like) fractures.

Paget's disease of bone (PDB) is the second most common bone disease mostly developing after 50 years of age at one or more localized skeletal sites; it is associated with severely high bone turnover, bone enlargement, bowing/deformity, cracking, and pain. Here, to specifically address the origins of the deteriorated mechanical integrity, we use a cohort of control and PDB human biopsies to investigate multiscale architectural and compositional modifications to the bone structure (ie, bone quality) and relate these changes to mechanical property measurements to provide further insight into the clinical manifestations (ie, deformities and bowing) and fracture risk caused by PDB. Here, at the level of the collagen and mineral (ie, nanometer-length scale), we find a 19% lower mineral content and lower carbonate-to-phosphate ratio in PDB, which accounts for the 14% lower stiffness and 19% lower hardness promoting plastic deformation in pathological bone. At the microstructural scale, trabecular regions are known to become densified, whereas cortical bone loses its characteristic parallel-aligned osteonal pattern, which is replaced with a mosaic of lamellar and woven bone. Although we find this loss of anisotropic alignment produces a straighter crack path in mechanically-loaded PDB cases, cortical fracture toughness appears to be maintained due to increased plastic deformation. Clearly, the altered quality of the bone structure in PDB affects the mechanical integrity leading to complications such as bowing, deformities, and stable cracks called fissure fractures associated with this disease. Although the lower mineralization and loss of aligned Haversian structures do produce a lower modulus tissue, which is susceptible to deformities, our results indicate that the higher levels of plasticity may compensate for the lost microstructural features and maintain the resistance to crack growth.

Data acquired from synchrotron-based X-ray computed tomography provide complete descriptions of the stochastic positions of each fiber in large bundles within composite samples. The data can be accumulated for distances along the nominal fiber direction that are long enough to reveal meandering or misalignment. Data are analyzed for a single fiber bundle consolidated as a mini-composite specimen and a block of fibers embedded within a single ply in a tape laminate specimen. The fibers in these materials differ markedly in their departure from alignment and the patterns formed by fiber deviations. The tape laminate specimen exhibits evidence of fibers that have slipped laterally through the bundle in narrow shear bands, which may be a mechanism of bundle deformation under transverse compression and shear. This pattern is absent in the single-tow specimen, which was not subject to transverse loads in processing. We propose a combination of topological and Euclidean metrics to quantify these and other stochastic bundle characteristics. Topological metrics are based on the neighbor map of fibers, which is constructed on cross-sections of the bundle by Delaunay triangulation (or Voronoi tessellation). Variations of the neighbor map along the fiber direction describe fiber meandering, twist, etc. Euclidean metrics include factors such as local fiber density and fiber orientation. The metrics distinguish bundle types, enable quantification of the effects of the manufacturing history of bundles, and provide target statistics to be matched by virtual specimens that might be generated for use in fiber-scale virtual tests.

Through a process called perilacunar remodeling, bone-embedded osteocytes dynamically resorb and replace the surrounding perilacunar bone matrix to maintain mineral homeostasis. The vital canalicular networks required for osteocyte nourishment and communication, as well as the exquisitely organized bone extracellular matrix, also depend upon perilacunar remodeling. Nonetheless, many questions remain about the regulation of perilacunar remodeling and its role in skeletal disease. Here, we find that suppression of osteocyte-driven perilacunar remodeling, a fundamental cellular mechanism, plays a critical role in the glucocorticoid-induced osteonecrosis. In glucocorticoid-treated mice, we find that glucocorticoids coordinately suppress expression of several proteases required for perilacunar remodeling while causing degeneration of the osteocyte lacunocanalicular network, collagen disorganization, and matrix hypermineralization; all of which are apparent in human osteonecrotic lesions. Thus, osteocyte-mediated perilacunar remodeling maintains bone homeostasis, is dysregulated in skeletal disease, and may represent an attractive therapeutic target for the treatment of osteonecrosis.

The multiscale hierarchical structure of bone is naturally optimized to resist fractures. In osteogenesis imperfecta, or brittle bone disease, genetic mutations affect the quality and/or quantity of collagen, dramatically increasing bone fracture risk. Here we reveal how the collagen defect results in bone fragility in a mouse model of osteogenesis imperfecta (oim), which has homotrimeric α1(I) collagen. At the molecular level, we attribute the loss in toughness to a decrease in the stabilizing enzymatic cross-links and an increase in nonenzymatic cross-links, which may break prematurely, inhibiting plasticity. At the tissue level, high vascular canal density reduces the stable crack growth, and extensive woven bone limits the crack-deflection toughening during crack growth. This demonstrates how modifications at the bone molecular level have ramifications at larger length scales affecting the overall mechanical integrity of the bone; thus, treatment strategies have to address multiscale properties in order to regain bone toughness. In this regard, findings from the heterozygous oim bone, where defective as well as normal collagen are present, suggest that increasing the quantity of healthy collagen in these bones helps to recover toughness at the multiple length scales.

Laboratory diffraction contrast tomography (LabDCT) enables a user to reconstruct 3D grain maps of polycrystalline materials non-destructively. For each grain, the morphology and crystallographic orientation, as well as derived properties such as grain boundary properties can be determined. Through two application examples this paper demonstrates the capabilities and potential of the current LabDCT implementation. Firstly, for well-annealed grain structures the reproducibility of LabDCT for more than 95% of the grains was found to be 5 μm on grain center-of-mass positions and 0.02° on orientations, while 90% of the grain boundary locations are determined with an accuracy better than 4 μm. The second example highlights the available statistics on thousands of grains, as well as the complementarity between LabDCT and absorption contrast tomography, readily available due to the integration of LabDCT on a commercial X-ray microscope

The processing of ceramic scaffolds using the ice-templating, or freeze casting, technique provides a relatively simple means to mimic the hierarchical design of natural materials such as nacre. In the present study, we investigated the architecture of silicon carbide (SiC) scaffolds produced by this technique over a range of cooling rates and suspension characteristics to demonstrate its versatility and effectiveness for fabricating unidirectional porous bodies with controlled lamella thickness, porosity fraction and morphology. An array of microstructures was generated specifically to examine the role of the suspension solid load and cooling rate on the pore morphology and final ceramic fraction. With respect to the morphology of the pores, a transition from lamellar to dendritic structure was found to be triggered by an increase in cooling rate or in suspension concentration. Similarly, the freezing condition and suspension characteristics were seen to influence the transition between particle rejection and entrapment by the ice. Based on this study, the specific processing parameters that result in distinct scaffold morphologies, namely lamellar, dendritic or isotropic morphology (the latter corresponding to particle entrapment), are identified and presented in the form of a “morphology map” to establish the regions of the different architectures of freeze-cast SiC scaffolds.

Techniques for characterizing tow architectures and defects in woven ceramic composites are required for generating high-fidelity geometric models and subsequently probing effects of defects on composite performance. Although X-ray computed tomography (CT) has been shown to provide the requisite information with potentially sub-μm resolution, the technique is inherently limited to probing only small volumes: on the order of a few unit cells of typical weaves. Here, we present an assessment of the efficacy of a complementary 2D technique, based on surface topography mapping via 3-D (three-dimensional) digital image correlation (DIC), with potential for ascertaining long-range features in weaves and defects that cannot be gleaned from CT imaging alone. Upon comparing surfaces reconstructed from CT and DIC data, we find that DIC is capable of resolving surface heights with a root mean square(RMS) error of ~10 μm (about twice the CT voxel size, 4.4 μm) and a spatial resolution of ~20 μm over areas of several cm2. Achieving this level of resolution requires use of sufficiently small speckles (~50 μm) and small subset size (~300 μm) relative to the characteristic tow dimensions (~1 mm). The error is somewhat higher (about 20 μm) in areas where surface discontinuities or rapid changes in topography exist (e.g., at tow boundaries).

Ceramic matrix composites are the emerging material of choice for structures that will see temperatures above ~1,500 °C in hostile environments, as for example in next-generation gas turbines and hypersonic-flight applications. The safe operation of applications depends on how small cracks forming inside the material are restrained by its microstructure. As with natural tissue such as bone and seashells, the tailored microstructural complexity of ceramic matrix composites imparts them with mechanical toughness, which is essential to avoiding failure. Yet gathering three-dimensional observations of damage evolution in extreme environments has been a challenge. Using synchrotron X-ray computed microtomography, we have fully resolved sequences of microcrack damage as cracks grow under load at temperatures up to 1,750 °C. Our observations are key ingredients for the high-fidelity simulations used to compute failure risks under extreme operating conditions.

Synchrotron micro tomography was used to identify the failure process and damage mechanisms during in - situ compressive loading on confined silica sand. In these tomography experiments, sand grains were confined inside a polycarbonate tube. These confined sand grains were loaded under strain control using a custom built X-ray imaging compatible load frame. The behavior of sand under increasing strain was observed in - situ with 23.8 keV X-rays and spatial resolution 1.45 μm/pixel. A software procedure was developed for processing the reconstructed data and for visualizing and understanding crack propagation in the sand grains. Deformation modes were observed macroscopically across many grains and microscopically within the grains. On the scale of a few sand grains, observations showed deformation effects such as preferred orientation of grains along which stresses were transferred. On a microscopic scale, micro-cracking within individual grains was followed by fragmentation of individual sand grains. Over a maximum applied strain of 34% on the column, the observed deformations were localized within a near-field comprising the top 60% of the sand volume.

Recent work presented a Monte Carlo algorithm based on Markov Chain operators for generating replicas of textile composite specimens that possess the same statistical characteristics as specimens imaged using high resolution x-ray computed tomography. That work represented the textile reinforcement by one-dimensional tow loci in three-dimensional space, suitable for use in the Binary Model of textile composites. Here analogous algorithms are used to generate solid, three-dimensional (3D) tow representations, to provide geometrical models for more detailed failure analyses. The algorithms for generating 3D models are divided into those that refer to the topology of the textile and those that deal with its geometry. The topological rules carry all the information that distinguishes textiles with different interlacing patterns (weaves, braids, etc.) and provide instructions for resolving interpenetrations or ordering errors among tows. They also simplify writing a single computer program that can accept input data for generic textile cases. The geometrical rules adjust the shape and smoothness of the generated virtual specimens to match data from imaged specimens. The virtual specimen generator is illustrated using data for an angle interlock weave, a common 3D textile architecture.

A Monte Carlo algorithm is defined for generating replicas of textile composite specimens that possess the same statistical characteristics as specimens imaged using high resolution computed tomography. The textile reinforcement is represented by one-dimensional tow loci in three-dimensional space, which are easily incorporated into the Binary Model of textile composites. A tow locus is expressed as the sum of non-stochastic, periodic variations in the coordinates of the tow centroid and stochastic, non-periodic deviations. The non-stochastic variations have period commensurate with the dimensions of the unit cell of the textile, while the stochastic deviations, which describe geometrical defects, exhibit correlation lengths that may be incommensurate with the unit cell. The model is calibrated with data deduced in prior work from computed tomography images. The calibration obviates the need for assuming any ideal shape functions for the tow loci, which can take very general form. The approach is therefore valid for a wide range of textile architectures. Once calibrated, a Markov Chain algorithm can generate numerous stochastic replicas of a textile architecture very rapidly. These virtual specimens can be much larger than the real specimens from which the data were originally gathered, a necessary feature when real specimen size is limited by the nature of high resolution computed tomography. The virtual specimen generator is illustrated using data for an angle interlock weave.