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All sourcesNASA NTRSDOE OSTI
NASA NTRSDate not supplied

Synchrotron Tomography of SiC/SiC Minicomposites to Observe and Quantify Damage Evolution

Composite performance is dictated by its microstructure – property relationships. For example, the characteristic response of ceramic matrix composites (CMCs) depends on the distribution of its constituents (i.e. fibers, matrix, fiber coatings, matrix cracks, and voids). Micro x-ray computed tomography (micro-CT) provides an opportunity to characterize the distribution of these constituents and to quantify the CMC microstructure in three-dimensions. To this end, In-situ micro-CT was performed at the Advanced Light Source (ALS) in combination with uniaxial tensile testing on SiC/SiC minicomposites. This work will describe the tensile load-dependent damage evolution within the microstructure of the SiC/SiC CMC specimens. The results from the micro-CT datasets can be used to develop micromechanical models that effectively capture damage initiation and progression in CMCs. In addition, details regarding the segmentation tools and techniques employed to understand and quantify these large tomography datasets will be presented.

Ashley Hilmas↗
NASA NTRS2017

In-Situ Observations of Longitudinal Compression Damage in Carbon-Epoxy Cross Ply Laminates Using Fast Synchrotron Radiation Computed Tomography

The role of longitudinal compressive failure mechanisms in notched cross-ply laminates is studied experimentally with in-situ synchrotron radiation based computed tomography. Carbon/epoxy specimens loaded monotonically in uniaxial compression exhibited a quasi-stable failure process, which was captured with computed tomography scans recorded continuously with a temporal resolutions of 2.4 seconds and a spatial resolution of 1.1 microns per voxel. A detailed chronology of the initiation and propagation of longitudinal matrix splitting cracks, in-plane and out-of-plane kink bands, shear-driven fiber failure, delamination, and transverse matrix cracks is provided with a focus on kink bands as the dominant failure mechanism. An automatic segmentation procedure is developed to identify the boundary surfaces of a kink band. The segmentation procedure enables 3-dimensional visualization of the kink band and conveys the orientation, inclination, and spatial variation of the kink band. The kink band inclination and length are examined using the segmented data revealing tunneling and spatial variations not apparent from studying the 2-dimensional section data.

Bergan, Andrew C.↗
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 NTRS2015

Analysis of Fibrous Felts for Flexible Ablators Using Synchrotron Hard X-Ray Micro-Tomography

We analyzed the material properties of low-density felts that are used as substrates for new-generation flexible and conformal carbon/phenolic ablators, and compared them with those of a rigid carbon fiber preform that is used to manufacture rigid carbon/phenolic ablators. Micro-tomography measurements were obtained using synchrotron X-rays, allowing the characterization of the materials microstructure at the scale of the fibers. Using the tomography voxels as computational grids, we computed tortuosity and room temperature conductivity. In addition we performed micro-scale simulations of the oxidation of carbon fibers using a random walk model for oxygen diffusion and a probability law to model surface reactions.

Ablation↗
NASA NTRSDate not supplied

Direct Measurement of the Composition of Aqueous Fluids from the Parent Body of Asteroid 162173 Ryugu

Imaging using X-ray absorption contrast by synchrotron nano-computed tomography (47.4 nm/voxel, 7keV) of a Ryugu pyrrhotite crystal (C0002-FC012-from the second touch-down site) revealed probable fluid inclusions (Fig. 1A,B) [1]. The inclusions were completely encapsuled in pyrrhotite, suggesting the fluids were trapped in the early stages of crystal growth, and filled with low-Z material. We performed Time-of Flight-Secondary Ion Mass Spectrometry (TOF-SIMS) depth profiling and high-resolution map-ping at -120°C to exposure and measure the composition of the trapped fluids in a frozen state.

M Zolensky↗
NASA NTRSDate not supplied

Update on Measurement of the Composition of Ryugu Fluid Inclusions

Imaging using X-ray absorption contrast by synchrotron nano-computed tomography of a Ryugu pyrrhotite crystal (C0002-FC012 - from the second Hayabusa2 spacecraft touch-down site) revealed probable fluid inclusions in the center of a crystal of pyrrhotite, suggesting the parent fluids were trapped in the early stages of crystal growth on Ryugu’s parent asteroid. We previously described the performance of Time-of Flight-Secondary Ion Mass Spectrometry (TOF-SIMS) depth profiling and high-resolution mapping at -120°C to expose and measure the composition of the trapped fluids in a frozen state in two Ryugu inclusions [1,2]. Here we report results from follow-on measurements of additional inclusions in the same pyrrhotite crystal, and the initial results of measurement of standards. The ultimate goal is to reveal the quantitative composition of the fluids that caused aqueous alteration, in particular the H2O:CO2 ratio, which will also facilitate cosmochemical modeling of the alteration process.

M Zolensky↗
NASA NTRS2023

Direct Analyses of Aqueous Fluids from C-Class Asteroid 162173 Ryugu

Imaging using X-ray absorption contrast by synchrotron nano-computed tomography (47.4 nm/voxel, 7keV) of a Ryugu pyrrhotite crystal revealed probable fluid inclusions. The inclusions were completely encapsuled in pyrrhotite, suggesting the fluids were trapped in the early stages of crystal growth, and filled with low-Z material. We performed Time-of Flight-Secondary Ion Mass Spectrometry (TOF-SIMS) depth profiling and high-resolution mapping at -120°C to exposure and measure the composition of the trapped fluids in a frozen state. These measurements revealed that the ancient, trapped fluids on Ryugu’s parent asteroid were saline aqueous solutions containing H2O, CO2, sulfur species, and nitrogen- and chlorine-bearing organic compounds identified by representative secondary ion species including O(-), OH(-), CO(-), S(-), Cl(-), C2(-), C2H(-), and CN(-). The inferred presence of CO2 indicates formation of the sulfides, and by implication the Ryugu parent body, beyond the H2O and CO2 snow lines of the early solar system, i.e. > 3-4 au from the Sun.

M Zolensky↗
NASA NTRS2023

Fluid Inclusions in Extraterrestrial Samples: Failures, Successes, Possibilities, and A Note of Caution

Over the past half century the search for life in the solar system and beyond has become a major research focus, with much effort devoted to finding evidence for liquid H2O and reduced carbon-bearing (organic) species in extraterrestrial samples. The most direct and convincing evidence for the presence of water and organic molecules is provided by fluid inclusions (FI)trapped in minerals that formed on the parent bodies. Beginning in the 1970s, reports of FI in extraterrestrial samples generated much enthusiasm within the planetary sciences community. However, many of the reported FI were determined to be artifacts of sample preparation, or incomplete characterization of features that appear to be FI, or were inconsistent with the inferred PT history of the meteorite sample. An early report of aqueous (and hydrocarbon-bearing) FI in stony meteorites and the subsequent follow-up study that showed that most or all of the “FI” contained water used during cutting and polishing of the samples led to a general unwillingness to believe later reports of FI in meteorites. One of the first confirmed occurrences of extraterrestrial aqueous (liquid) fluid inclusions in a meteorite was reported by Zolensky et al. (1999; Science), who described aqueous inclusions in halite in the Monahans and later the Zag meteorites. These meteorite falls were collected shortly after landing on earth and were prepared without using water or other fluids that could introduce artifacts. The oxygen and hydrogen isotopic composition of water in FI in these same samples was later measured, showing that the fluids represent various degrees of water-rock interaction on the parent body .In more recent years, careful studies of FI trapped in extraterrestrial samples combining synchrotron X-ray computed tomography to locate FI in samples followed by cryo-TOF-SIMS analysis of the FI have identified the presence of molecular fragments suggesting the presence of H2O and various organic molecules in the fluids. Challenges associated with studying FI in extraterrestrial samples include the limited abundance of potential host phases for FI, such as carbonates and phosphates, the often poor optical quality of the host phases, and the small size of the FI, with few as large as 5 microns and most less than 1-2 microns in maximum dimension

Robert Bodnar↗
NASA NTRS1990

Synchrotron radiation - Applications in the earth sciences

Synchrotron-radiation sources and their characteristics are overviewed along with recent synchrotron-based research on earth materials and future earth-science applications utilizing the next generation of synchrotron-radiation sources presently under construction. Focus is placed on X-ray scattering studies of earth materials (crystalline and noncrystalline) under ambient conditions, diffraction studies of earth materials at high pressures and/or temperatures, spectroscopic studies, primarily X-ray absorption spectroscopy, and spatially resolved X-ray fluorescence studies of compositional variations in earth materials. It is noted that other synchrotron-based methods, such as X-ray tomography and topography may become important in characterizing earth materials, while soft X-ray/vacuum ultraviolet radiation from synchrotron sources can be applied to problems involving the structural environments of low-atomic-number elements and the characterization of surface reactions of minerals with liquids and gases.

Bassett, W. A.↗
NASA NTRS2017

Effect of Tube-Based X-Ray Microtomography Imaging on the Amino Acid and Amine Content of the Murchison CM2 Chondrite

X-ray and synchrotron X-ray micro-computed tomography (micro-CT) are increasingly being used for three dimensional reconnaissance imaging of chondrites and returned extraterrestrial material prior to detailed chemical and mineralogical analyses. Although micro-CT imaging is generally considered to be a non-destructive technique since silicate and metallic minerals in chondrites are not affected by X-ray exposures at the intensities and wavelengths typically used, there are concerns that the use of micro-CT could be detrimental to the organics in carbonaceous chondrites. We recently conducted a synchrotron micro-CT experiment on a powdered sample of the Murchison CM2 carbonaceous chondrite exposed to a monochromatic high energy (approximately 48 kiloelectronvolts) total X-ray radiation dose of approximately 1 kilogray (kGy) using the Advanced Photon Source beamline 13-BMD (13-Bending Magnet-D Beamline) at Argonne National Laboratory and found that there were no detectable changes in the amino acid abundances or enantiomeric compositions in the chondrite after exposure relative to a Murchison control sample that was not exposed. However, lower energy bremsstrahlung X-rays could interact more with amino acids and other lower molecular weight amines in meteorites. To test for this possibility, three separate micro-CT imaging experiments of the Murchison meteorite using the GE Phoenix v/tome/x s 240 kilovolt microfocus high resolution tungsten target X-ray tube instrument at the American Museum of Natural History (AMNH) were conducted and the amino acid abundances and enantiomeric compositions were determined. We also investigated the abundances of the C1-C5 amines in Murchison which were not analyzed in the first study.

Microtomography Imaging↗
NASA NTRS2017

A New Method of Absorption-Phase Nanotomography for 3D Observation of Mineral-Organic-Water Textiles and its Application to Pristine Carbonaceous Chondrites

Pristine carbonaceous chondrites contain fine-grained matrix, which is composed largely of amorphous silicates, sub-micron silicate and sulfide crystals, and organic materials. They are regarded as primitive dust in the early Solar System that have suffered minimal alteration in their parent bodies. The matrix generally has different lithologies; some of them are unaltered but some are more or less aqueously altered. Their textures have been examined in 2D usually by FE-SEM/EDS, TEM/EDS, nano-SIMS and micro-XRD. Observation of their complex fine textures, such as spatial relation between different lithologies in 3D, is important for understanding aggregation and alteration processes. Synchrotron radiation (SR)-based X-ray tomography reveals 3D structures nondestructively with high spatial resolution of approximately greater than 100 nm. We have developed a new technique using absorption contrasts called "dual-energy tomography" (DET) to obtain 3D distribution of minerals at SPring-8, SR facility in Japan, and applied successfully to Itokawa particles. Phase and absorption contrast images can be simultaneously obtained in 3D by using "scanning-imaging x-ray microscopy" (SIXM) at SPring-8, which can discriminate between void, water and organic materials. We applied this technique combined with FIB micro-sampling to carbonaceous chondrites to search for primitive liquid water. In this study, we combined the DET and SIXM to obtain three dimensional submicron-scale association between minerals, organic materials and water and applied this to pristine carbonaceous chondrites.

Tsuchiyama, A.↗
NASA NTRS2016

From Tomography to Material Properties of Thermal Protection Systems

The X-ray micro-tomography technique provides non-destructive characterizations of three-dimensional material micro-structures at spatial resolutions from the sub-micron to the centimeter scale. High quality micro-tomography images of NASA Thermal Protection System (TPS) materials are obtained using one of the brightest synchrotron X-ray sources available. Leveraging on NASA supercomputing capabilities, material properties and response are computed from tomography-data. This talk highlights the process and challenges of going from 3D images of actual material structures to simulations of properties and phenomena relevant to TPS material response, such as thermal conductivity, permeability, mass transport and high temperature reactions. The talk is addressed to a broad audience including scientists, engineers, researchers, educators, programmers, managers, and members of the media.

tomography↗
NASA NTRS2010

Search for Organic Nanoglobules in Carbonaceous Chondrites Using Microtomography

Primitive solar materials have various organic matters. In recent years, novel organic materials called organic nanoglobules of a few hundred micrometers in typical size were discovered in carbonaceous chondrites, IDPs, and comet 81P/Wild 2. The organic globules are spherical shape and in many cases with hollow structures. Composition of the globules are mainly aromatic carbon. The isotopic anomalies of SD and 6N 15 observed in the globules indicate that they were formed from photochemical reaction to ice particles at very low temperature environment, such as molecular clouds or outer protosolar disk. Aqueous alteration of organic matters and the gamma-ray irradiation to PAH are also suggested as alternative possible formation processes. If the globules are made from organic ice particles, the hollow regions of the globules are suggested to be once filled with volatile H20-rich organic ices, while if they were formed by aqueous alteration, the hollow regions should be filled with a fluid which caused the aqueous alteration. However, fluids in the globules have not been detected so far in the previous studies. If fluids were originally preserved in the hollows, they might be lost during destructive processes of sample separation or preparation for TEM observation. X-ray computed tomography (CT) is a nondestructive method which can determine 3-D internal structures of objects. SR (synchrotron radiation)-based imaging microtomography can give submicron spatial resolution [8] and was applied to micro textures in extraterrestrial materials, such as cometary grains captured by the Stardust mission [9]. If organic globules are observed non-destructively in carbonaceous chondrites by tomography, we can check the presence of fluids in the hollows. If fluids are preserved, we may analyze chemical and isotopic compositions of the fluids. The purpose of this study is to observe organic nanoglobules using imaging tomography for future analysis.

Matsumoto, T.↗
NASA NTRS2024

X-Ray Micro- and Nano-Tomography Analysis of Bennu Samples: A Preliminary Report

X-ray tomography (XCT) is an effective technique for obtaining the 3D structures of returned samples. XCT using synchrotron radiation provides high-resolution CT images with quantitative information. The XCT systems at SPring-8, an SR facility in Japan, have been used to analyze samples returned from the asteroids Itokawa and Ryugu. In this study, we plan to apply SR-XCT to samples returned from the asteroid Bennu.

A Tsuchiyama↗
NASA NTRS2019

3d Crystallographic Orientation of Olivine in Bjurböle Chondrules

The crystallographic orientations of chondrule minerals can provide important insights into their formation and deformational history. For example, the orientations of the olivine bars and surrounding rim in barred olivine chondrules provide information and on the conditions of crystallization and the orientations and shapes of olivines within porphritic chondrules can record the reactions with the surrounding nebular gas during chondrule formation. Later deformation on the parent body can cause crystal-plastic deformation of chondrule minerals that is evident through their intracrystalline lattice misorientations. Typically these crystal orientations and lattice misorientations are determined using electron backscatter diffraction (EBSD) on thin sections but this gives only a 2D picture for what is actually a 3D texture. While it is possible to combine EBSD with serial sectioning to build a 3D dataset of texture, this is a destructive, time-intensive process. A recent technological development that enables non-destructive, 3D crystallographic orientation measurement is X-ray diffraction contrast tomography (DCT), which uses the X-ray diffraction of the crystal lattice to determine orientation. Originally only possible using monochromatic X-ray beams at 3rd generation synchrotron light sources, DCT has been recently adapted to polychromatic sources of laboratory X-ray microscopes (referred to as Lab-DCT). Up to this point LabDCT has only been applied to large, well-formed crystals of high symmetry (i.e., metals), but we recently acquired DCT datasets for a pair Bjurböle chondrules to determine the applicability of the technique to natural, mutlimineralic samples composed predominately of olivine (i.e., chondrules).

Hanna, R. D.↗
NASA NTRS2017

3-D-Observation of Matrix of MIL 090657 Meteorite by Absorption-Phase Tomography

MIL 090657 meteorite (CR2.7) is one of the least altered primitive carbonaceous c hondrites [1]. This meteorite has amorphous silicates like GEMS (glass with embedded metal and sulfide), which are characteristically contained in cometary dust, in matrix [2,3] as with the Paris meteorite [4]. Three lithologies have been recognized; lithology-1 (L 1) dominated by submicron anhydrous silicates, lithology-2 (L2) by GEMS-like amorphous silicates and lithology-3 (L3) by phyllosilicates [2]. Organic materials are abundant in L 1 and L2 [2,3]. L 1 and L2 were further divided into sub-lithology respectively based on their textures and compositions [5]. These studies were performed by 2D SEM and TEM observations of sample surfaces and thin sections that are unable to reveal what constitute each lithology and how these lithologies are distributed and related to each other. This information will provide important insights into alteration and aggregation processes on asteroids and in the early solar nebula. In this study, MIL 090657 matrix was examined in 3D using two types of X-ray tomography; DET (dual-energy tomography) [6] and SIXM (scanning-imaging X-ray microscopy) [7]. Mineral phases can be discriminated based on absorption contrasts at two different X-ray energies in DET. In SIXM, materials composed of light elements such as water or organic materials can be identified based on phase and absorption contrasts. By combining these methods, we can discriminate not only organic materials from voids but also hydrous alteration products, such as hydrated silicates and carbonates, from anhydrous minerals [8]. In this study, we first observed cross sections of MIL 090657 matrix fragments C1 00 mm) in detail using FE-SEM/ EDS. Based on the results, three house-shaped samples (3 0 -50 mm) were extracted from L 1, L2 and their boundary (H1, H3 and H5, respectively) using FIB. 3D imaging of these samples were conducted at BL47XU of SPring-8, a synchrotron radiation facility, with -30-40 nm/ voxel and - 70-80 nm/ voxel at 7keV and 8keV in DET and -100 nm/ voxel at 8keV in SIXM. We found new lithologies that we named L4, L5 and L6 in H1 and H3 in addition to L 1 and L2. L4. L5 and L6 are mainly composed of probably phyllosilicates with different Fe contents. Sulfide and framboidal magnetite were recognized in L4. L5 includes magnetite and carbonate and L6 includes anhydrous silicates having cracks inside. L 1, L2, L4 and L5 are porous while few voids were observed in L6. L4 adjoins to L 1 with boundary, which is not very distinct. L2, L5 and L6 adjoin to each other, and the boundaries of L6 with L2 and L5 are clear. In H5, coarse mineral grains C5-1 0 mm) such as Fe-metal and enstatite are present in L 1 and L2. L 1-L2 boundary is not sharp in 3 D. In conclusion, we found a variety of lithologies by 3D observation for the first time, suggesting that t he MIL 0 90657 meteorite experienced complex alteration and aggregation histories. As L2 is dominated by amorphous silicates, which are extremely susceptible to aqueous alteration, t his is p resumed to be t he most primitive lithology. The contact between L2 and phyllosilicate-bearing lithologies (L5 and L6) with clear boundaries indicates that they were aggregated after aqueous alteration of L5 and L6. The indistinct boundary between L 1 and L2 is suggesting that these two lithologies might originally be the same aggregate composed of amorphous silicates and coarse mineral grains. L 1 might have experienced weak aqueous alteration followed by mild thermal alteration [2], while L2 did not undergo aqueous alteration.

Miyama, Sugimoto↗