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X-Ray Microtomography Measurements of Coevolving Particle Size and Shape

This study measures simultaneous changes in particle size and shape during grain crushing and proposes quantitative metrics to track their coevolving statistical distribution. Idealized granular materials with widely different initial particle shapes (i.e., spheres, quasi-ellipsoids, plates, and rods) are compressed oedometrically at vertical stress levels sufficient to induce particle breakage. X-ray microtomography and digital image analysis are then used to track changes in particle-scale characteristics. The observations indicate that more irregular particles tend to exhibit a higher degree of breakage compared to more spherical grains subjected to an equivalent stress level. Despite these differences, the measurements also indicate that all the tested particle sets approach a common attractor (expressed in terms of aspect ratio, flatness, and elongation), regardless of their initial morphology. A new shape evolution index is proposed to quantify such trends. With this new metric, it is shown that in all the tested materials, the particle shape evolves faster than size, especially for the more regular morphologies, thus implying that the shape tends to reach its attractor point before the grading reaches its ultimate particle size distribution. Furthermore, this finding underpins an ultimate stage of crushing-driven compression that occurs with particle size reduction but minimal shape changes (i.e., self-replicating shapes due to fractures).

Oedometric compression↗

The strain-dependent spatial evolution of garnet in a high- P ductile shear zone from the Western Gneiss Region (Norway): a synchrotron X-ray microtomography study

Reaction and deformation microfabrics provide key information to understand the thermodynamic and kinetic controls of tectono-metamorphic processes, however they are usually analysed in two dimensions, omitting important information regarding the third spatial dimension. We applied synchrotron-based X-ray microtomography to document the evolution of a pristine olivine gabbro into a deformed omphacite-garnet eclogite in four dimensions, where the 4th dimension is represented by the degree of strain. In the investigated samples, which cover a strain gradient into a shear zone from the Western Gneiss Region (Norway), we focused on the spatial transformation of garnet coronas into elongated clusters of garnets with increasing strain. Our microtomographic data allowed quantification of garnet volume, shape and spatial arrangement evolution with increasing strain. We combined microtomographic observations with light microscope- and backscatter electron images as well as electron microprobe- (EMPA) and electron backscatter diffraction (EBSD) analysis to correlate mineral composition and orientation data with the X-ray absorption signal of the same mineral grains. With increasing deformation, the garnet volume almost triples. In the low strain domain, garnets form a well interconnected large garnet aggregate that develops throughout the entire Page 1 of 52 sample. We also observed that garnet coronas in the gabbros never completely encapsulate olivine grains. In the most highly deformed eclogites, the oblate shapes of garnet clusters reflect a deformational origin of the microfabrics. We interpret the aligned garnet aggregates to direct synkinematic fluid flow and consequently influence the transport of dissolved chemical components. EBSD analyses reveal that garnet show a near-random crystal preferred orientation that testifies no evidence for crystal plasticity. There is, however evidence for minor fracturing, neo-nucleation and overgrowth. Microprobe chemical analysis revealed that garnet compositions progressively equilibrate to eclogite facies, becoming more almandine-rich. We interpret these observations as pointing to a mechanical disintegration of the garnet coronas during strain localisation, and their rearrangement into individual garnet clusters through a combination of garnet coalescence and overgrowth while the rock was deforming.

garnet↗

Quantifying Mesoscale Neuroanatomy Using X-Ray Microtomography

Methods for resolving the three-dimensional (3D) microstructure of the brain typically start by thinly slicing and staining the brain, followed by imaging numerous individual sections with visible light photons or electrons. In contrast, X-rays can be used to image thick samples, providing a rapid approach for producing large 3D brain maps without sectioning. Here we demonstrate the use of synchrotron X-ray microtomography (µCT) for producing mesoscale (~1 µm 3 resolution) brain maps from millimeter-scale volumes of mouse brain. We introduce a pipeline for µCT-based brain mapping that develops and integrates methods for sample preparation, imaging, and automated segmentation of cells, blood vessels, and myelinated axons, in addition to statistical analyses of these brain structures. Our results demonstrate that X-ray tomography achieves rapid quantification of large brain volumes, complementing other brain mapping and connectomics efforts.

60 APPLIED LIFE SCIENCES↗

Density of NaAlSi 2 O 6 Melt at High Pressure and Temperature Measured by In-Situ X-ray Microtomography

In this study, the volumetric compression of jadeite (NaAlSi 2 O 6 ) melt at high pressures was determined by three-dimensional volume imaging using the synchrotron-based X-ray microtomography technique in a rotation-anvil device. Combined with the sample mass, measured using a high-precision analytical balance prior to the high-pressure experiment, the density of jadeite melt was obtained at high pressures and high temperatures up to 4.8 GPa and 1955 K. The density data were fitted to a third-order Birch-Murnaghan equation of state, resulting in a best-fit isothermal bulk modulus K T0 of $10.8$ $^{+1.9}_{–5.3}$ GPa and its pressure derivative K' T0 of $3.4$ $^{+6.6}_{–0.4}$. Comparison with data for silicate melts of various compositions from the literature shows that alkali-rich, polymerized melts are generally more compressible than alkali-poor, depolymerized ones. The high compressibility of jadeite melt at high pressures implies that polymerized sodium aluminosilicate melts, if generated by low-degree partial melting of mantle peridotite at ~250–400 km depth in the deep upper mantle, are likely denser than surrounding mantle materials, and thus gravitationally stable.

36 MATERIALS SCIENCE↗

Mafic explosive volcanism at Llaima Volcano: 3D x-ray microtomography reconstruction of pyroclasts to constrain shallow conduit processes

Abstract Mafic volcanic activity is dominated by effusive to mildly explosive eruptions. Plinian and ignimbrite-forming mafic eruptions, while rare, are also possible; however, the conditions that promote such explosivity are still being explored. Eruption style is determined by the ability of gas to escape as magma ascends, which tends to be easier in low-viscosity, mafic magmas. If magma permeability is sufficiently high to reduce bubble overpressure during ascent, volatiles may escape from the magma, inhibiting violent explosive activity. In contrast, if the permeability is sufficiently low to retain the gas phase within the magma during ascent, bubble overpressure may drive magma fragmentation. Rapid ascent may induce disequilibrium crystallization, increasing viscosity and affecting the bubble network with consequences for permeability, and hence, explosivity. To explore the conditions that promote strongly explosive mafic volcanism, we combine microlite textural analyses with synchrotron x-ray computed microtomography of 10 pyroclasts from the 12.6 ka mafic Curacautín Ignimbrite (Llaima Volcano, Chile). We quantify microlite crystal size distributions (CSD), microlite number densities, porosity, bubble interconnectivity, bubble number density, and geometrical properties of the porous media to investigate the role of magma degassing processes at mafic explosive eruptions. We use an analytical technique to estimate permeability and tortuosity by combing the Kozeny-Carman relationship, tortuosity factor, and pyroclast vesicle textures. The groundmass of our samples is composed of up to 44% plagioclase microlites, > 85% of which are < 10 µm in length. In addition, we identify two populations of vesicles in our samples: (1) a convoluted interconnected vesicle network produced by extensive coalescence of smaller vesicles (> 99% of pore volume), and (2) a population of very small and completely isolated vesicles (< 1% of porosity). Computed permeability ranges from 3.0 × 10 −13 to 6.3 × 10 −12 m 2 , which are lower than the similarly explosive mafic eruptions of Tarawera (1886; New Zealand) and Etna (112 BC; Italy). The combination of our CSDs, microlite number densities, and 3D vesicle textures evidence rapid ascent that induced high disequilibrium conditions, promoting rapid syn-eruptive crystallization of microlites within the shallow conduit. We interpret that microlite crystallization increased viscosity while simultaneously forcing bubbles to deform as they grew together, resulting in the permeable by highly tortuous network of vesicles. Using the bubble number densities for the isolated vesicles (0.1-3 −3 × 10 4 bubbles per mm 3 ), we obtain a minimum average decompression rate of 1.4 MPa/s. Despite the textural evidence that the Curacautín magma reached the percolation threshold, we propose that rapid ascent suppressed outgassing and increased bubble overpressures, leading to explosive fragmentation. Further, using the porosity and permeability of our samples, we estimated that a bubble overpressure > 5 MPa could have been sufficient to fragment the Curacautín magma. Other mafic explosive eruptions report similar disequilibrium conditions induced by rapid ascent rate, implying that syn-eruptive disequilibrium conditions may control the explosivity of mafic eruptions more generally.

Valdivia, Pedro↗

Poisson’s ratio of eTPU molded bead foams in compression via in situ synchrotron X-ray microtomography

In situ synchrotron X-ray microtomography was used to characterize the bulk deformation behavior by computing the Poisson's ratio of expanded thermoplastic polyurethane (eTPU) molded bead foams used in footwear midsole during compression. Quantitative data on morphological characteristics were obtained using an iterative image processing workflow. Image correlation on the 4D datasets using DVC was performed to calculate the volumetric and axial strain to estimate the Poisson ratio. Strain maps from DVC showed the influence of variability in ligament thickness distribution on the global mechanical behavior exhibited which dominated the response seen in these bead foams. Lastly, our results showed a strong correlation between Poisson ratio and distribution of ligament thickness in foams.

36 MATERIALS SCIENCE↗

Deformation and fracture behavior of a laser powder bed fusion processed stainless steel: In situ synchrotron x-ray computed microtomography study

Tensile plastic deformation and fracture behavior of a laser powder bed fusion processed 316L stainless steel alloy was investigated in situ using high-resolution synchrotron x-ray computed microtomography (sXCT). Three different cases were studied: (1) specimen A1, near full-density with initial porosity of 0.04%, (2) specimen B1, initial lack-of-fusion (LOF) porosity of about 3% with the major axis of defects aligned nearly perpendicular to the tensile loading direction (LD), and (3) specimen B, similar to B1 but with the major axis of LOF defects aligned nearly parallel to LD. The effects of type, density, and orientation of defects in as-printed samples on plastic deformation and failure modes were studied by analyzing sXCT image sequences and quantitative defect properties. Specifically, the evolutions of porosity, size, aspect ratio, and angle of gas pores and LOF defects were characterized as a function of applied strain. Moreover, interactions between as-printed defects and deformation-induced crack propagation were investigated. The tensile behavior of specimen A1 was comparable to that of a commercial wrought plate. Furthermore, the quantitative in-situ sXCT results showed a void-growth phenomenon in A1 but without noticeable coalescence, resulting in a ductile cup-cone failure. Specimen B1 showed damage-driven brittle failure with limited plasticity due to early and rapid propagation of open voids. On the other hand, specimen B, with a similar amount of LOF defects as B1, showed deceivingly strong and ductile tensile behavior similar to A1 without any major crack propagations due to the favorable orientation relationship between LOF defects and the LD.

36 MATERIALS SCIENCE↗

Quantitative characterization of soil micro-aggregates: New opportunities from sub-micron resolution synchrotron X-ray microtomography

Soil microaggregates are the fundamental building block, at the micron scale, of the highly hierarchical structure of soils, and can exert a significant control on the local biological metabolism and microbial community partitioning. In this study we propose an analysis protocol for the morphometric characterization of complete soil microaggregates based on sub-micron resolution synchrotron X-ray microtomography. A comprehensive characterization of the aggregate morphology is the first step towards a complete characterization of the soil microaggregates, when trying to correlate morphometric parameters with physical and/or biological properties, or when building models (e.g., effective diffusivity, microbial distribution, etc.). In this study, we demonstrate our characterization approach on two single microaggregate samples from dramatically different soil environments: one from Kansas, primarily composed by inorganic particles, and one from Barrow (Alaska) dominated by plant fragments. A series of state-of-the-art morphometric analysis techniques have been employed providing quantitative results highlighting specific differences of the two samples. The role of the microstructure in a scenario microbial population development has been discussed and it has been found that the Barrow microaggregate seems to be more favorable, from a purely geometrical point of view, as also confirmed by a simple model presented in this work. Finally, the potential of this approach, when coupled with chemical and biological analysis for a fully comprehensive characterization of soil aggregates in the larger picture of enhanced biological activity, is evident.

54 ENVIRONMENTAL SCIENCES↗

Comparing the Purity of Rolled versus Evaporated Lithium Metal Films Using X-ray Microtomography

Here, we present a comparison of lithium metal films produced via rolling and thermal evaporation using synchrotron hard X-ray microtomography. In past studies of rolled lithium metal foils, a large number of C, O, and N impurities were found and identified as the key cause for failure in lithium metal cells. In this comparison, the X-ray tomography data show that the evaporated lithium metal films have an average impurity concentration of 19 particles/mm3 in comparison to 1350 particles/mm3 in the rolled lithium metal. An analysis of the inner substrate/lithium interface and outer lithium surface of the thermally evaporated film shows a much greater concentration of impurities at these interfaces, further emphasizing the importance of interface engineering in producing high-quality lithium metal batteries. Furthermore, we show that, if surface contamination can be avoided, it is possible to obtain lithium films with no impurities detectable by synchrotron hard X-ray tomography.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

In Situ Visualization of Li-Whisker with Grating-Interferometry-Based Tricontrast X-ray Microtomography

The lithium-ion battery has demonstrated tremendous economic and social impacts. Upon battery operation under different conditions, lithium changes its chemical state and physical formation, leading to undesired side reactions, e.g., lithium dendrite growth that degrades the cell performance and causes safety concerns. In situ detection and visualization of lithium metal in functional batteries could offer insights with both scientific and industrial significance but remain a frontier challenge. In this work, we demonstrate in situ three-dimensional imaging of lithium whisker using a grating-interferometry-based tricontrast X-ray microtomography method. Our approach explicitly reveals the micromorphology of the electrochemically developed porous lithium whisker with micrometer-level spatial resolution while offering sensitivity to the nanoporosity that is smaller than the nominal resolution limit. Our result reveals valuable structural information on the lithium whisker that is otherwise inaccessible. This method is also readily applicable to a broad range of battery research, including all-solid-state batteries.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

A novel technique for investigation of complete and partial anisotropic wetting on structured surface by X-ray microtomography

An experimental study about the anisotropic wetting behavior of a surface patterned with parallel grooves is presented as an application example of a novel technique for investigation of complete and partial anisotropic wetting on structured surface by X-ray microtomography. Shape of glycerin droplets on such surface is investigated by X-ray micro computed tomography (microCT) acting as a non-intrusive, full volume 3D microscope with micrometric spatial resolution. The reconstructed drop volumes enable to estimate the exact volumes of the drops, their base contours, and 3D static contact angles, based on true cross-sections of the drop-surface couple. Droplet base contours are compared to approximate geometrical contour shapes proposed in the literature. Contact angles along slices parallel and perpendicular to the grooves direction are compared with each other. The effect of the sessile drop volume on the wetting behavior is discussed. The proposed technique, which is applicable for any structured surface, enables the direct measure of Wenzel ratio based on the microCT scan in the wetted region usually inapproachable by any others. Comparisons with simplified models are presented and congruence of results with respect to the minimum resolution needed is evaluated and commented.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Recent progress of hard x-ray imaging microscopy and microtomography at BL37XU of SPring-8

A hard x-ray imaging microscopy and microtomography system is now being developed at the beamline 37XU of SPring-8. In the latest improvement, a spatial resolution of about 50 nm is achieved in two-dimensional imaging at 6 keV x-ray energy using a Fresnel zone plate objective with an outermost zone width of 35 nm. In the tomographic measurement, a spatial resolution of about 100 nm is achieved at 8 keV using an x-ray guide tube condenser optic and a Fresnel zone plate objective with an outermost zone width of 50 nm.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Equally sloped X-ray microtomography of living insects with low radiation dose and improved resolution capability

Three-dimensional X-ray imaging of living specimens is challenging due to the limited resolution of conventional absorption contrast X-ray imaging and potential irradiation damage of biological specimens. In this letter, we present microtomography of a living specimen combining phase-contrast imaging and a Fourier-based iterative algorithm termed equally sloped tomography. Non-destructive 3D imaging of an anesthetized living yellow mealworm Tenebrio molitor was demonstrated with a relatively low dose using synchrotron generated X-rays. Based on the high-quality 3D images, branching tracheoles and different tissues of the insect in a natural state were identified and analyzed, demonstrating a significant advantage of the technique over conventional X-ray radiography or histotomy. Additionally, the insect survived without problem after a 1.92-s X-ray exposure and subsequent absorbed radiation dose of ∼1.2 Gy. No notable physiological effects were observed after reviving the insect from anesthesia. The improved static tomographic method demonstrated in this letter shows advantage in the non-destructive structural investigation of living insects in three dimensions due to the low radiation dose and high resolution capability, and offers many potential applications in biological science.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

A compact and flexible induction furnace for in situ X-ray microradiograhy and computed microtomography at Elettra: design, characterization and first tests

A compact and versatile induction furnace for in situ high-resolution synchrotron and laboratory hard X-ray microradiography and computed microtomography is described. The furnace can operate from 773 to 1723 K. Its programmable controller enables the user to specify multiple heating and cooling ramp rates as well as variable dwell times at fixed temperatures allowing precise control of heating and cooling rates to within 5 K. The instrument can work under a controlled atmosphere. Thanks to the circular geometry of the induction coils, the heat is homogeneously distributed in the internal volume of the graphite cell ( ca . 150 mm 3 ) where the sample holder is located. The thermal gradient within the furnace is less than 5 K over a height of ca . 5 mm. This new furnace design is well suited to the study of melting and solidification processes in geomaterials, ceramics and several metallic alloys, allowing fast heating (tested up to 6.5 K s -1 ) and quenching (up to 21 K s -1 ) in order to freeze the sample microstructure and chemistry under high-temperature conditions. The sample can be held at high temperatures for several hours, which is essential to follow phenomena with relatively slow dynamics, such as crystallization processes in geomaterials. The utility of the furnace is demonstrated through a few examples of experimental applications performed at the Elettra synchrotron laboratory (Trieste, Italy).

Kudrna Prašek, Marko↗

Focused‐beam X‐ray fluorescence and diffraction microtomographies for mineralogical and chemical characterization of unsectioned extraterrestrial samples

Abstract This study describes the application of new synchrotron X‐ray fluorescence (XRF) and diffraction (XRD) microtomographies for the 3‐D visualization of chemical and mineralogical variations in unsectioned extraterrestrial samples. These improved methods have been applied to three compositionally diverse chondritic meteorite samples that were between 300 and 400 μm in diameter, including samples prepared from fragments of the CR2 chondrite LaPaz Icefield (LAP) 02342, H5 chondrite MacAlpine Hills (MAC) 88203, and the CM2 chondrite Murchison. The synchrotron‐based XRF and XRD tomographies used are focused‐beam techniques that measure the intensities of fluorescent and diffracted X‐rays in a sample simultaneously during irradiation by a high‐energy microfocused incident X‐ray beam. Measured sinograms of the emitted and diffracted intensities were then tomographically reconstructed to generate 2‐D slices of XRF and XRD intensity through the sample, with reconstructed pixel resolution of 1–2 μm, defined by the resolution of the focused incident X‐ray beam. For sample LAP 02342, primary mineral phases that were visualized in reconstructed slices using these techniques included isolated grains of α‐Fe, orthopyroxene, and olivine. For our sample of MAC 88203, XRF/XRD tomography allowed visualization of forsteritic olivine as a primary mineral phase, a vitrified fusion crust at the sample surface, identification of localized Cr‐rich spinels at spatial resolutions of several micrometers, and imaging of a plagioclase‐rich glassy matrix. In the sample of Murchison, major identifiable phases include clinoenstatite‐ and olivine‐rich chondrules, variable serpentine matrix minerals and small Cr‐rich spinels. Most notable in the tomographic analysis of Murchison is the ability to quantitatively distinguish and visualize the complex mixture of serpentine‐group minerals and associated tochilinite–cronstedtite intergrowths. These methods provide new opportunities for spatially resolved characterization of sample texture, mineralogy, crystal structure, and chemical state in unsectioned samples. This provides researchers an ability to characterize such samples internally with minimal disruption of sample micro‐structures and chemistry, possibly without the need for sample extraction from some types of sampling and capture media.

Geochemistry & Geophysics↗

Technical Note: Synchrotron-based high-energy x-ray phase sensitive microtomography for biomedical research

Purpose: Propagation-based phase-contrast CT (PPCT) utilizes highly sensitive phase-contrast technology applied to x-ray microtomography. Performing phase retrieval on the acquired angular projections can enhance image contrast and enable quantitative imaging. In this work, the authors demonstrate the validity and advantages of a novel technique for high-resolution PPCT by using the generalized phase-attenuation duality (PAD) method of phase retrieval. Methods: A high-resolution angular projection data set of a fish head specimen was acquired with a monochromatic 60-keV x-ray beam. In one approach, the projection data were directly used for tomographic reconstruction. In two other approaches, the projection data were preprocessed by phase retrieval based on either the linearized PAD method or the generalized PAD method. The reconstructed images from all three approaches were then compared in terms of tissue contrast-to-noise ratio and spatial resolution. Results: The authors’ experimental results demonstrated the validity of the PPCT technique based on the generalized PAD-based method. In addition, the results show that the authors’ technique is superior to the direct PPCT technique as well as the linearized PAD-based PPCT technique in terms of their relative capabilities for tissue discrimination and characterization. Conclusions: This novel PPCT technique demonstrates great potential for biomedical imaging, especially for applications that require high spatial resolution and limited radiation exposure.

60 APPLIED LIFE SCIENCES↗

Structure of a Deformed Inhomogeneous Material on the Data of Acoustic Emission and X-Ray Computer Microtomography

Accumulation of defects at various stages of the deformation of a structurally inhomogeneous material (granite) has been studied using two nondestructive methods: acoustic emission (AE) and X-ray computer microtomorgaphy (CT). The quasi-static testing of cylindrical samples of a Westerly granite was carried out under uniaxial compression. The control of the defect formation was realized using the real-time monitoring of acoustic emission. For each sample under study, several steps of the loading and tomographic imaging have been performed. We have found that an exponential or power-law function of the energy distribution of the AE signals makes it possible to select a sample region, in which the system of defects has transited into a self-organized criticality state and large cracks have been formed. This result coincides with the data of the X-ray tomography Computer Microtomography.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Lithium-Sulfur Batteries with a Block Copolymer Electrolyte Analyzed by X-ray Microtomography

Most of the work on Lithium-sulfur (LiS) batteries use liquid electrolytes that have limited stability when coupled with Li metal anodes. We have studied LiS batteries with a solid block copolymer electrolyte which exhibits improved stability against Li anodes. Additionally, the electrolyte comprises a polystyrene-b-poly(ethylene oxide) (SEO) copolymer doped with a Li salt. Hollow carbon nanospheres impregnated with sulfur were used to build a composite cathode. Two types of sulfur-impregnated functionalized carbon nanospheres were used: One with carboxylic acid groups and the other with short lithium poly(4-styrenesulfonyl(trifluoromethylsulfonyl)imide) (PSTFSI-Li) chains. Cells with Li S dissolved in the SEO based electrolyte served as the baseline. After cycling, the reason for capacity fade was determined by imaging the batteries using synchrotron hard X-ray microtomography. It is generally assumed that LiS cells fail due to dissolution of polysulfide into the liquid electrolyte, i.e., the main problems related to the cathode. In our all-solid cells, failure was primarily due to delamination of the Li foil from the polymer electrolyte layer. Delamination is also observed at the sulfur cathode. It is likely that the large changes in volume of the active materials during cycling induce delamination in all-solid LiS cells. 2 8

25 ENERGY STORAGE↗