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At least 19 records
All sourcesNASA NTRSDOE OSTI
DOE OSTI2025

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↗
NASA NTRS2015

Effect of a Synchrotron X-ray Microtomography Imaging Experiment on the Amino Acid Content of a CM Chondrite

X-ray microcomputed tomography and synchrotron X-ray microcomputed tomography (μCT) are becoming popular tools for the reconnaissance imaging of chondrites. However, there are occasional concerns that the use of μCT may be detrimental to organic components of a chondrite. Soluble organic compounds represent ~2–10% of the total solvent extractable carbon in CI and CM carbonaceous chondrites and amino acids are among the most abundant compounds in the soluble organic fraction. We irradiated two samples of the Murchison CM2 carbonaceous chondrite under conditions slightly harsher (increased beam exposure time) than those typically used for x-ray μCT imaging experiments to determine if detectable changes in the amino acid abundance and distribution relative to a nonexposed control sample occurred. After subjecting two meteorite portions to ionizing radiation dosages of 1.1 kiloGray (kGy) and 1.2 kGy with 48.6 and 46.6 keV monochromatic X-rays, respectively, we analyzed the amino acid content of each sample. Within analytical errors, we found no differences in the amino acid abundances or enantiomeric ratios when comparing the control samples (nonexposed Murchison) and the irradiated samples. We show with calculations that any sample heating due to x-ray exposure is negligible. We conclude that a monochromatic synchrotron X-ray μCT experiment at beamline 13-BM-D of the Advanced Photon Source, which imparts ~1 kGy doses, has no detectable effect on the amino acid content of a carbonaceous chondrite. These results are important for the initial reconnaissance of returned samples from the OSIRIS-REx and Hayabusa 2 asteroid sample return missions.

Jon M. Friedrich↗
NASA NTRS2011

Three Dimensional Structures of Particles Recovered from the Asteroid Itokawa by the Hayabusa Mission and a Role of X-Ray Microtomography in the Preliminary Examination

Particles of regolith on S-type Asteroid 25143 Itokawa were successfully recovered by the Hayabusa mission of JAXA (Japan Aerospace Exploration Agency). Near-infrared spectral study of Itokawa s surface indicates that these particles are materials similar to LL5 or LL6 chondrites. High-resolution images of Itokawa's surface suggest that they may be breccias and some impact products. At least more than 1500 particles were identified as Itokawa origin at curation facility of JAXA. Preliminary analysis with SEM/EDX at the curation facility shows that they are roughly similar to LL chondrites. Although most of them are less than 10 micron in size, some larger particles of about 100 micron or larger were also identified. A part of the sample (probably several tens particles) will be selected by Hayabusa sample curation team, and sequential examination will start from January 2011 by Hayabusa Asteroidal Sample Preliminary Examination Team (HASPET). In mainstream of the analytical flow, each particle will be examined by microtomography, XRD and XRF first as nondestructive analyses, and then the particle will be cut by an ultra-microtome and examined by TEM, SEM, EPMA, SIMS, PEEM/XANES, and TOF-SIMS sequentially. Three-dimensional structures of Itokawa particles will be obtained by microtomography sub-team of HASPET. The results together with XRD and XRF will be used for design of later destructive analyses, such as determination of cutting direction and depth, to obtain as much information as possible from small particles. Scientific results and a role of the microtomography in the preliminary examination will be presented.

Tsuchiyama, A.↗
DOE OSTI2025

Characterizing the pore-scale impacts of enhanced-solubilization solutions on organic-liquid morphology and fluid-fluid interfacial area with microtomography

Synchrotron X-ray microtomography was used to directly quantify the impact of enhanced-solubilization solutions on mobilization of a non-wetting fluid in a natural porous medium. Polyoxyethylene sorbitan monooleate (tween 80), hydroxypropyl-β-cyclodextrin (HPCD), sodium dodecyl sulfate (SDS), and ethanol were used as the solubilization reagents. Tetrachloroethene (PCE) was used as the entrapped organic immiscible liquid. Microtomography images were collected prior to and after successive floods with each reagent solution. The total trapping number was varied by more than three orders of magnitude by changing the velocity and viscosity of the aqueous phase as well as the interfacial tension between fluid phases. The results were compared to those obtained from equivalent experiments conducted with water flooding. Inspection of images indicated that mobilization caused a change in PCE morphology and distribution for all reagents with the exception of HPCD, for which a lower trapping number was determined compared to the other experiments. Mobilization of organic liquid was observed at total trapping numbers that were consistent with prior work. The enhanced-solubilization solutions had minimal impact on the configuration or magnitude of fluid-fluid interfacial area.

Interfacial area↗
NASA NTRS1990

The metrology of spherical shells using synchrotron x ray microtomography

With recent advances in solid state imaging technology and the increasing availability of synchrotron x-ray radiation sources, synchrotron x-ray microtomography is emerging as a nondestructive technique for the evaluation of the structure and composition of small specimens with spatial resolution in the micron range. Synchrotron radiation offers the following advantages over conventional x-ray sources: high brightness, continuous emission which is tunable over a large energy range, faster data collection rates, and a highly collimated beam of large cross section permitting the illumination of large specimens. Synchrotron x-ray microtomography enables the structure of individual spheres to be evaluated in order to reveal the concentricity and sphericity of the internal void and the uniformity of the shell wall in the case of high quality spherical shells for Sandia National Laboratories' Inertial Confinement Fusion project.

Hmelo, Anthony B.↗
NASA NTRS2006

Effect of 16-Day Spaceflight on the Morphology of Thick-Toed Geckos (Pachydactylus Bibronii Smith, 1846)

There are grounds to believe that space flown experiments on thick-toed geckos may help solve the problem of floatation of vertebrates in microgravity. Geckos of this species carry on the lower surface of their toes numerous setae, which allow them to remain attached to any surfaces regardless of the gravitational effects. Experiments were performed on 5 animals in each of the following groups: flight, basal, synchronous and laboratory controls. 32 hours after a 16- day flight the animals were euthanazed and examined using traditional histology and X-ray microtomography. Body mass losses were 10% in the flight animals, 7.4% in the synchronous controls, and 12.3% in the laboratory controls. Since the flight and synchronous animals were kept at 15-19 C, whereas the laboratory controls - at 26-28 C, it can be inferred that environmental temperatures impacted animal metabolism no less than flight induced stress. Blood tests of the flown animals showed a 12% decrease of erythrocytes and a 40% decrease of dark-nuclear granulocytes, with the number of light-nuclear granulocytes remaining unchanged. In the small intestine the number of goblet cells increased allowing them to occupy a large portion of the cyptal surface. Enhanced secretion was accompanied by the appearance of dead intestinal cells in the lumen. Clusters of degraded hepatocytes were found at the liver edges of flight animals. Signs of liver involution were similar to the changes produced by alcohol consumption but did not spread to its central part. In the heart, insignificant hypertrophy and excessive blood supply that still remained within the physiological norm were detected. No significant changes were found in the pancreas, lungs, nervous systems or the snouts of the flown animals, but the volume of their gallbladders was greater than in controls. The epithelium of toe pads of the flight animals became thinner. Histological examination of the humerus did not demonstrate significant mineral losses. However, X-ray microtomography showed changes in the trabecular structure in the subepyphyseal zone of bones in flight animals compared to the controls. In summary, all the changes detected in the flight animals were adaptive. Therefore, geckos of this species can be used as an animal model for morphological studies in longer-duration space flights.

Gulimova, V. I.↗
DOE OSTI2025

Carbon Fiber Oxidation in 4D

The oxidation of carbon fibers at high temperatures is the primary degradation process in the thermal protection system of many hypersonic flight vehicles. Predicting the rate and the extent of oxidation is critical to ensure a safe and effective design. An oversized thermal protection system adds unnecessary mass, while an under-designed one risks system failure and mission loss. Resolving high-temperature material degradation due to oxidation has been a long-standing challenge in designing for re-entry flight environments. Using time-resolved in situ X-ray microtomography, the oxidation of carbon fibers at high temperatures is directly imaged, resolving the two limiting degradation regimes: diffusion- and reaction-limited. The ability to resolve material degradation in time at the sub-micron scale sheds light on the ablation phenomenon and enables predictions of material constitutive properties evolving in time, with profound implications on the ability to model the aerothermal response of heat shield materials in hostile environments.

ablation↗
DOE OSTI2026

Establishing the Stability of Cross-Linked Poly(ethylene oxide) Blended with Poly(pentyl malonate) against Lithium Metal Anodes

This work focuses on an electrolyte obtained by infusing linear poly(pentyl malonate) (PPM) chains into cross-linked poly(ethylene oxide) (PEO). A lithium salt is added to enable ion transport. Obtaining this electrolyte is only possible because PPM is miscible with PEO irrespective of salt concentration. The properties of this electrolyte are compared against two benchmarks: an electrolyte obtained by infusing linear PEO into cross-linked PEO and cross-linked PEO with no added linear polymer. Measurements of storage moduli and ion transport efficacies are found to be similar across the three electrolytes, suggesting similar stability behavior against lithium metal anodes, based on current theoretical models. Instead, the PPM infused electrolyte outperforms the other two electrolytes. In the cycling tests, the current supported by the PPM infused electrolyte was a factor of 20 higher than that of the PEO infused electrolyte and a factor of 4 higher than that of the cross-linked PEO electrolyte. In the unidirectional plating experiments, the other two electrolytes fail after about 4 h or less, while the PPM containing electrolyte did not fail during the 140 h testing period. Insight into the nature of failure modes was obtained using synchrotron hard X-ray microtomography.

Gido, Lily [University of California, Berkeley]↗
DOE OSTI2025

Fluid/Fluid Interfacial Areas Measured for Different Non-Wetting/Wetting Fluid Pairs in Natural Porous Media

This study examined the impact of fluid type and grain diameter on the interfacial area between different pairs of non-wetting and wetting fluids in natural porous media. Synchrotron X-ray microtomography was used to obtain high-resolution, three-dimensional images of multi-phase porous media systems. Multiple porous media, comprising a range of physical and geochemical properties, were used in this study. The four pairs of non-wetting/wetting fluids used were dense OIL/water, light OIL/water, air/dense OIL, and air/water. Images were obtained over a broad range of wetting phase saturation and for both wetting phase drainage and imbibition conditions. The results showed that for each fluid pair, the total (capillary + film) interfacial area increased with decreasing wetting fluid saturation. Interfacial areas were similar among all fluid pairs for a given porous medium. They were also similar for drainage and imbibition conditions. The maximum specific interfacial area (A m ) was shown to correlate well with inverse median grain diameter. The physical properties of the porous medium appear to have a greater influence on the magnitude of specific total interfacial area for a given saturation than fluid properties or wetting phase history.

NAPL↗
NASA NTRS1990

Regional distribution of mineral and matrix in the femurs of rats flown on Cosmos 1887 biosatellite

The location and nature of the defect in mineralization known to occur in growing animals after spaceflight are studied. The distribution of bone mineral density in situ is mapped, and these images are correlated with the chemical composition of the diaphyseal bone. Concentrations of mineral and osteocalcin are found to be low in the distal half of the diaphysis and concentrations of collagen to be low with evidence of increased synthesis in the proximal half of the diaphysis of the flight bones. X-ray microtomography indicates a longitudinal gradient of decreasing mineralization toward the distal diaphysis. Analysis of embedded sections by backscattered electrons reveals patterns of mineral distribution in the proximal, central, and distal regions of the diaphysis and also shows a net reduction in mineral levels toward the distal shaft. Increases in mineral density to higher fractions in controls are less in the flight bones at all three levels.

Mechanic, Gerald L.↗
DOE OSTI2025

Effect of bisphosphonate treatment on the oim mouse middle ear ossicles' structure, composition and hearing

Hearing loss is common in people with osteogenesis imperfecta (OI or brittle bone disease). Bisphosphonates are commonly used to treat long bone fragility in children with OI. However, its impact on the bone quality of the middle ear ossicles and hearing remains unknown. This study determines whether bisphosphonates treatment itself may contribute to hearing loss in OI by evaluating its effects in the oim/oim mouse model of severe OI having normal auditory function. Specifically, this study reports the effects of alendronate (ALN), a nitrogen-containing bisphosphonate, on ossicle morphology, porosity, and elemental composition in 14-week-old oim/oim mice treated weekly, starting at 2 weeks of age. The ossicles were examined using synchrotron microtomography and X-ray fluorescence microscopy (XFM). Hearing was assessed longitudinally until 26 weeks of age by determining auditory brainstem response (ABR) thresholds in another group of mice also treated weekly starting at 2 weeks of age. ALN treatment further reduces in size the already small oim/oim ossicles, specifically in female mice. Porosity, bone composition, and hearing function, however, were generally not affected by the ALN treatment. Furthermore, ALN does not prevent joint fusions, excessive bone formations, or enlarged joint spaces in WT or oim/oim experimental groups. One ALN-treated oim/oim mouse with a bone formation in the interior of the footplate, and one ALN-treated WT mouse with a fixed footplate had frequency-specific hearing loss. Since footplate abnormalities are not observed in PBS-treated mice in this study, it remains unclear whether ALN fails to prevent these changes or contributes to their development. Future studies should investigate the mechanisms of ossicular abnormalities and bisphosphonates modulatory role in the ossicles.

60 APPLIED LIFE SCIENCES↗
DOE OSTI2024

Fracture Dynamics in Silicon Anode Solid-State Batteries

Solid-state batteries (SSBs) with silicon anodes could enable improved safety and energy density compared to lithium-ion batteries. However, degradation arising from the massive volumetric changes of silicon anodes during cycling is not well understood in solid-state systems. Here, we use operando X-ray computed microtomography to reveal micro- to macro-scale chemo-mechanical degradation processes of silicon anodes in SSBs. Mud-type channel cracks driven by biaxial tensile stress form across the electrode during delithiation. We also find detrimental cracks at the silicon/ solid electrolyte interface that form due to local reaction competition between neighboring domains of different sizes. Continuum phase-field damage modeling quantifies stress-driven channel cracking and shows that the lithiated silicon stress state is critical for determining the extent of interfacial fracture. This work reveals the mechanisms that govern SSBs compared to conventional lithium-ion batteries and provides guidelines for engineering chemomechanically resilient electrodes for high-energy batteries.

25 ENERGY STORAGE↗
DOE OSTI2025

Physical properties, internal structure, and the three‐dimensional petrography of CI chondrites

physical properties and the nature of their breccation, we investigated nine samples of the Ivuna and Orgueil CI chondrites ranging in size from 1 mm to 4 cm in approximate diameter. The combined mass of unique material investigated in this work is 113 g. For our investigations, we use ideal gas pycnometry, 3-D laser scanning, x-ray computed microtomography (μCT), and accompanying digital data extraction techniques. We found that the bulk density of the samples ranged from 1.61 to 2.10 g cm −3 . Larger samples tend to have a lower bulk density. Grain density (ranging from 2.44 to 2.55 g cm −3 ) is significantly less variable than the bulk density in our samples and the quantity of porosity (ranging from 14.6% to 33.8%) is the dominant factor in determining the bulk density of CI chondrite material. Our μCT results show that the visible porosity across all sizes of our CI chondrite samples is in the form of cracks, but these cracks can account for less than two-thirds of the porosity in the CI chondrites. Other porosity is not visible, even at μCT resolutions of 2.7 μm voxel edge −1 and we conclude that it is sub-micron in nature. It is not clear if the cracks seen in our samples are indigenous to the chondrites or are a result of terrestrial processes. We also find that the CI chondrites are excellent examples of the fractal-like nature of brecciation, where clasts can be observed at all scales we imaged. The breccias are composed of sub-equant-shaped and sub-rounded-textured clasts like melt-free impact breccias on other solar system bodies. From our μCT volume and digital data extraction, we determine that the Ivuna CI chondrite breccia is organized: the mostly sub-equant clasts within our ~2 cm chunk of Ivuna have a mean diameter of 1.33 mm and their aligned longest axes define a lineation structure. We speculate that the lineation was imparted after fragmentation of the clasts by slight shear on the parent asteroid which could be the result of seismic-related granular flow or mild non-axial impact-related compaction. These data will help to place returned asteroidal material from asteroids 162173 Ryugu and 101955 Bennu and the CI chondrites into a mutual geological context.

CI chondrite↗
NASA NTRS2008

Three-Dimensional Shapes and Impactor Size Estimation of Stardust Impact

Impact tracks formed by cometary dust capture in silica aerogel collectors in the Stardust mission [1] have a variety of shapes, showing diversity of the cometary dust [2]. We have investigated 3-D structures and elemental distributions of three impact tracks using synchrotron radiation x-ray analyses (microtomography and XRF) as one of the preliminary examination [3]. In this study, additional five tracks were investigated by the same analytical method. Impactor sizes of the tracks were estimated from the track entrance sizes and Fe abundances. Size parameters, such as length, of the tracks were normalized by the impactor size to compare track shape

Iida, Y.↗
NASA NTRS2015

Crystallography of Magnetite Plaquettes and their Significance as Asymmetric Catalysts for the Synthesis of Chiral Organics in Carbonaceous Chondrites

We have previously observed the magnetite plaquettes in carbonaceous chondrites using scanning electron microscope (SEM) imaging, examined the crystal orientation of the polished surfaces of magnetite plaquettes in CI Orgueil using electron backscattered diffraction (EBSD) analysis, and concluded that these magnetite plaquettes are likely naturally asymmetric materials. In this study, we expanded our EBSD observation to other magnetite plaquettes in Orgueil, and further examined the internal structure of these remarkable crystals with the use of X-ray computed microtomography.

Chan, Q. H. S.↗
NASA NTRS2008

Mineralogy, Three Dimensional Structure, and Oxygen Isotope Ratios of Four Crystalline Particles from Comet 81P/Wild 2

Preliminary examinations of small dust particles from comet 82P/Wild 2 revealed many expected and unexpected features. Among them the most striking feature is the presence of abundant crystalline material in the comet. Synchrotron radiation X-ray diffraction and microtomography are the most efficient methods to detect and describe bulk mineralogical features of crystalline cometary particles. In the present study, in addition to these two non-destructive techniques, electron microscopy and ion-probe mass spectrometry were carried out on the four crystalline particles.

Nakamura, T.↗
NASA NTRS2004

Sub-Micrometer Scale Minor Element Mapping in Interplanetary Dust Particles: A Test for Stratospheric Contamination

Combined X-ray microprobe (XRM), energy dispersive x-ray fluorescence using a Transmission Electron Microscope (TEM), and electron microprobe measurements have determined that the average bulk chemical composition of the interplanetary dust particles (IDPs) collected from the Earth s stratosphere is enriched relative to the CI meteorite composition by a factor of 2 to 4 for carbon and for the moderately volatile elements Na, K, P, Mn, Cu, Zn, Ga, Ge, and Se, and enriched to approximately 30 times CI for Br. However, Jessberger et al., who have reported similar bulk enrichments using Proton Induced X-ray Emission (PIXE), attribute the enrichments to contamination by meteor-derived atmospheric aerosols during the several weeks these IDPs reside in the Earth s atmosphere prior to collection. Using scanning Auger spectroscopy, a very sensitive surface analysis technique, Mackinnon and Mogk have observed S contamination on the surface of IDPs, presumably due to the accretion of sulfate aerosols during stratospheric residence. But the S-rich layer they detected was so thin (approximately 100 angstroms thick) that the total amount of S on the surface was too small to significantly perturb the bulk S-content of a chondritic IDP. Stephan et al. provide support for the contamination hypothesis by reporting the enrichment of Br on the edges of the IDPs using Time-of-Flight Secondary-Ion Mass-Spectrometry (TOFSIMS), but TOF-SIMS is notorious for producing false edge-effects, particularly on irregularly-shaped samples like IDPs. Sutton et al. mapped the spatial distribution of Fe, Ni, Zn, Br, and Sr, at the approximately 2 m scale, in four IDPs using element-specific x-ray fluorescence (XRF) computed microtomography. They found the moderately volatile elements Zn and Br, although spatially inhomogeneous, were not concentrated on the surface of any of the IDPs they examined, suggesting that the Zn and the Br enrichments in the IDPs are not due to contamination during stratospheric residence.

Flynn, G. J.↗
NASA NTRS2014

Search for Fluid Inclusions in a Carbonaceous Chondrite Using a New X-Ray Micro-Tomography Technique Combined with FIB Sampling

Early solar system aqueous fluids are preserved in some H chondrites as aqueous fluid inclusions in halite (e.g., [1]). Although potential fluid inclusions are also expected in carbonaceous chondrites [2], they have not been surely confirmed. In order to search for these fluid inclusions, we have developped a new X-ray micro-tomography technique combined with FIB sampling and applied this techniqu to a carbanaceous chondrite. Experimental: A polished thin section of Sutter's Mill meteorite (CM) was observed with an optical microscope and FE-SEM (JEOL 7001F) for chosing mineral grains of carbonates (mainly calcite) and sulfides (FeS and ZnS) 20-50 microns in typical size, which may have aqueous fluid inclusions. Then, a "house" similar to a cube with a roof (20-30 microns in size) is sampled from the mineral grain by using FIB (FEI Quanta 200 3DS). Then, the house was atached to a thin W-needle by FIB and imaged by a SR-based imaging microtomography system with a Fresnel zone plate at beamline BL47XU, SPring-8, Japan. One sample was imaged at two X-ray energies, 7 and 8 keV, to identify mineral phases (dual-enegy microtomography: [3]). The size of voxel (pixel in 3D) was 50-80 nm, which gave the effective spatial resolution of approx. 200 nm. A terrestrial quartz sample with an aqueous fluid inclusion with a bubble was also examined as a test sample by the same method. Results and discussion: A fluid inclusion of 5-8 microns in quartz was clearly identified in a CT image. A bubble of approx. 4 microns was also identified as refraction contrast although the X-ray absorption difference between fluid and bubble is small. Volumes of the fluid and bubble were obtained from the 3D CT images. Fourteen grains of calcite, two grains of iron sulfide and one grain of (Zn,Fe)S were examined. Ten calcite, one iron sulfide and one (Zn,Fe)S grains have inclusions >1 micron in size (the maximum: approx. 5 microns). The shapes are spherical or irregular. Tiny inclusions (<1 micron) are also present in all the grains examined. These results show that mineral grains have more inclusions than expected from 2D observations. The X-ray absorption of the inclusions shows that they are not solid inclusions. No bubbles were observed inside, indicating that we cannot determine whether they are really aqueous fluids or merely voids. One calcite grain has an inclusion approx. 2 microns in size, which seems to have a bubble and a tiny solid daughter crystal inside (three-phase inclusion). As we know the exact 3D position of the inclusion, we will anlyze the inclusion by SIMS after freezing the sample as has been done for a halite sample [3]. The present technique is useful for finding small inclusions not only in carbonaceous chondrites but also for terrestrial materials.

Tsuchiyama, A.↗