Search NASA⌕ Search

SEARCH · Search NASA

Results for “X-ray absorption fine structure”

Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

Quote a phrase for an exact phrase match. Source license links do not imply unrestricted reuse.

Applications of x ray absorption fine structure to the in situ study of the effect of cobalt in nickel hydrous oxide electrodes for fuel cells and rechargeable batteries

Electronic and structural aspects of composite nickel-cobalt hydrous oxides have been examined in alkaline solutions using in situ X-ray absorption fine structure (XAFS). The results obtained have indicated that cobalt in this material is present as cobaltic ions regardless of the oxidation state of nickel in the lattice. Furthermore, careful analysis of the Co K-edge Extended X-ray absorption fine structure data reveals that the co-electrodeposition procedure generates a single phase, mixed metal hydrous oxide, in which cobaltic ions occupy nickel sites in the NiO2 sheet-like layers and not two intermixed phases each consisting of a single metal hydrous oxide.

Kim, Sunghyun↗

Raman structural studies of the nickel electrode

The objectives of this investigation have been to define the structures of charged active mass, discharged active mass, and related precursor materials (alpha-phases), with the purpose of better understanding the chemical and electrochemical reactions, including failure mechanisms and cobalt incorporation, so that the nickel electrode may be improved. Although our primary tool has been Raman spectroscopy, the structural conclusions drawn from the Raman data have been supported and augmented by three other analysis methods: infrared spectroscopy, powder X-ray Diffraction (XRD), and x-ray absorption spectroscopy (in particular EXAFS, Extended X-ray Absorption Fine Structure spectroscopy).

Cornilsen, Bahne C.↗

Interdisciplinary research and development on the effects of the nature and properties of ceramic materials in the design of advanced structural components

An educational development and supportive research program on ceramic materials established to advance design methodology, improve materials, and develop engineers knowledgable in design with and use of high performance ceramic materials is described. Emphasis is on the structures and related materials problems in a ceramic turbine engine, but applications in coal gasification, solar conversion, and magnetohydrodynamic technologies are considered. Progress of various research projects in the areas of new materials, processing, characterization, and nondestructive testing is reported. Fracture toughness determination, extended X-ray absorption fine structure measurements, and grain boundary effects in beta-alumina are among the topics covered.

Source record↗

Iron impurities in Si3N4 processing

The atomic environment of iron impurities is investigated during the processing cycle of reaction-bonding silicon nitride (RBSN). Several analysis techniques are utilized, including X-ray photoelectron spectroscopy (XPS), extended X-ray absorption fine structure (EXAFS), and electron spin resonance (ESR), to examine iron impurities in the starting silicon powder, in sintered silicon compacts, and in RBSN materials. Results indicate that iron impurities in as-received metallurgical grade silicon powder are incorporated in the silicon bulk as a highly distorted FeSi2 compound. No surface iron or iron-based particulate is observed in the starting material. Upon sintering, the iron environment becomes an ordered FeSi2 structure. In the RBNS material, the FeSi2 structure is again distorted, as observed by both EXAFS and ESR.

Bouldin, C. E.↗

The nature of chemisorbed oxygen on Ni(100) and Cu(100)

Model calculations indicate two low-lying states for the interaction of O with Ni and Cu(100). The oxide state is approximately 1 eV more stable and its R(perpendicular) for Ni(100) is consistent with the experimental value for Ni(100), indicating only one type of stable chemisorption bond. This agrees with XPS (X-ray photoemission spectroscopy) and EXAFS (extended X-ray absorption fine structure) data for the observed LEED (low energy electron diffraction) structures. Interpretations of EELS (electron energy loss spectroscopy) data in terms of a radical state forthe p(2x2) and the oxide state for the c(2x2) structure must be seriously questioned.

Bauschlicher, C. W., Jr.↗

Studies of the Si/SiO2 interface using synchrotron radiation

Synchrotron radiation photoemission spectroscopy (SRPS) in the 1-4 KeV photon energy range is a useful tool for interface characterization. Results are presented of a series of studies of the near-interface region of Si/SiO2 which confirm that a bond strain gradient exists in the oxide as a result of lattice mismatch. These experiments include measurement of photoemission lineshape changes as a function of photon energy, corresponding changes in the electron escape depth near the interface, and surface extended X-ray absorption fine structure (SEXAFS) measurements directly indicating the shortening of the Si-Si second nearest neighbor distance in the near-interface region of the oxide.

Hecht, M. H.↗

Oxygen Fugacity of Mare Basalts and the Lunar Mantle Application of a New Microscale Oxybarometer Based on the Valence State of Vanadium

The ability to estimate oxygen fugacities for mare basalts and to extend these observations to the lunar mantle is limited using bulk analysis techniques based on buffering assemblages or the valence state of iron. These limitations are due to reequilibration of mineral assemblages at subsolidus conditions, deviations of mineral compositions from thermodynamic ideality, size requirements, and the limits of the iron valence at very low fO2. Still, these approaches have been helpful and indicate that mare basalts crystallized at fO2 between the iron-w stite buffer (IW) and the ilmenite breakdown reaction (ilmenite = rutile + iron). It has also been inferred from these estimates that the lunar mantle is also highly reduced lying at conditions below IW. Generally, these data cannot be used to determine if the mare basalts become increasingly reduced during transport from their mantle source and eruption at the lunar surface and if there are differences in fO2 among mare basalts or mantle sources. One promising approach to determining the fO2 of mare basalts is using the mean valence of vanadium (2+, 3+, 4+, 5+) determined on spots of a few micrometers in diameter using synchrotron x-ray absorption fine structure (XAFS) spectroscopy. The average valence state of V in basaltic glasses is a function of fO2, temperature, V coordination, and melt composition. Here, we report the initial results of this approach applied to lunar pyroclastic glasses.

Shearer, C. K.↗

On the determination of the origin of linear anomaly in the macrostructure of VPPA welded 2219-T87 aluminum alloy: Preliminary report

The cause and significance of the weld radiograph enigma, which is a linear anomaly in the features of the X-ray film is examined. By observing features on available radiographs and in studying published reports of similar features, it was possible to conclude that there are many manifestations of the enigma, and that they are all specific features of fine structure in radiographs due to natural processes connected with welding and to specific X-ray absorption and diffraction phenomena. These processes include the thermal distribution and liquid metal flow in welding, the development of microstructure, morphology, second phase particles and porosity due to the solidification process, and to the pattern of residual stresses after the weld metal has cooled to the ambient temperature. Microdensitometer traces were made across weld radiographs of standard enigmatic types. Similar patterns were produced by computer simulation. These show that the enigma is a relatively low contrast feature compared to real weld defects, such as undercuts or centerline cracks. The enigma can be distinguished from weld defects by these microdensitometer traces. The enigma effect on weld properties is not known but is expected to be minor.

Jemian, W. A.↗

On the determination of the origin of linear anomaly in the macrostructure of VPPA welded 2219-T87 aluminum alloy

The objective was to determine the cause and significance of the weld radiograph enigma, which is a linear anomaly in the features of the X-ray film. By observing features on available radiographs and in studying published reports of similar features it was possible to conclude that there are many manifestations of the enigma, and that they are all specific features of fine structure in radiographs due to natural processes connected with welding and to specific X-ray absorption and diffraction phenomena. These processes include the thermal distribution and liquid metal flow in welding, the development of microstructure, morpohology, second phase particles and porosity due to the solidification process and to the pattern of residual stresses after the weld metal has cooled to the ambient temperature. Microdensitometer traces were made across weld radiographs of standard and enigmatic types. Similar patterns were produced by computer simulation. These show that the enigma is a relatively low contrast feature compared to real weld defects, such as undercuts or centerline cracks. The enigma can be distinguished from weld defects by these microdensitometer traces. The enigma effect on weld properties is not known but is expected to be minor.

Jemian, W. A.↗

Effect of Scattering on Instabilities in Line-driven Stellar Winds

Line driven O-B stellar winds are unstable to perturbations of short spatial wavelength and the growth rates for such instabilities are very rapid. The nature of the nonlinear development of this instability is unknown, but might possibly be one of blobs of gas driven through ambient gas or a quasiregular train of outward moving shocks. In either case the resulting dissipation of mechanical energy might explain the observed anomalous heating n O-B stars as evidenced by their X-ray emission and high ionization state. It also might explain the observed fine structure of the absorption lines and their time variability. The driving due to the absorption of the stellar continuum flux was considered and the effects of the diffuse, scattered radiation field were neglected. It was shown that under certain special conditions the effect of scattering could reduce the instability growth rate to zero. A stability analysis that includes scattering, but that uses the more physically realistic assumption of complete redistribution instead of coherent scattering, and that includes the effects of transverse velocity gradients, which become important as the flow moves away from the stellar surface is presented. It is found that the instability is eliminated right at the base of the wind, but that as the flow moves outward the instability rate rapidly becomes equal to a substantial fraction of the calculated value, the fraction asymptotically reaching 80% at large radii. Since this still implies many e folds in a characteristic outflow time, the primary conclusion that these winds are highly unstable is unchanged.

Owocki, S. P.↗

Nustar Reveals an Intrinsically X-ray Weak Broad Absorption Line Quasar in the Ultraluminous Infrared Galaxy Markarian 231

We present high-energy (3-30 keV) NuSTAR observations of the nearest quasar, the ultraluminous infrared galaxy (ULIRG) Markarian 231 (Mrk 231), supplemented with new and simultaneous low-energy (0.5-8 keV) data from Chandra. The source was detected, though at much fainter levels than previously reported, likely due to contamination in the large apertures of previous non-focusing hard X-ray telescopes. The full band (0.5-30 keV) X-ray spectrum suggests the active galactic nucleus (AGN) in Mrk 231 is absorbed by a patchy and Compton-thin N(sub H) approx. 1.2(sup +0.3) sub-0.3) x 10(exp 23) / sq cm) column. The intrinsic X-ray luminosity L(sub 0.5-30 Kev) approx. 1.0 x 10(exp 43) erg /s) is extremely weak relative to the bolometric luminosity where the 2-10 keV to bolometric luminosity ratio is approx. 0.03% compared to the typical values of 2-15%. Additionally, Mrk 231 has a low X-ray-to-optical power law slope alpha(sub 0X) approx. -1.7. It is a local example of a low-ionization broad absorption line (LoBAL) quasar that is intrinsically X-ray weak. The weak ionizing continuum may explain the lack of mid-infrared [O IV], [Ne V], and [Ne VI] fine-structure emission lines which are present in sources with otherwise similar AGN properties. We argue that the intrinsic X-ray weakness may be a result of the super-Eddington accretion occurring in the nucleus of this ULIRG, and may also be naturally related to the powerful wind event seen in Mrk 231, a merger remnant escaping from its dusty cocoon.

Reveals↗

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.↗

Reflectivity Around the Gold M-Edges of X-ray Reflector of the Soft X-Ray Telescope Onboard ASTRO-H

The X-ray astronomy satellite ASTRO-H are equipped with two equivalent soft X-ray telescopes (SXT-I and SXT-S) which cover the energy band 0.3-12 keV. The X-ray reflectors of the SXTs are coated with a gold monolayer by means of the replication technique. A series of gold M absorption edges in the 2-4 keV band causes complex structures in the energy response of the SXTs. In the same band, there are astrophysically important emission lines from Si, Ar and S. Since the SXS has unprecedentedly high spectral resolution, we have measured the reflectivity around the gold M-edges in an extremely fine energy pitch at the synchrotron radiation facility KEK PF BL11-B, with the 2 eV pitch in 2100 eV to 4100 eV band that covers the entire series of the absorption edges (M-I through M-V) at grazing incident angles to the reflectors of 0.5, 0.8, 1.0, 1.2, 1.4 degree, and with a finer pitch of 0.25 eV in the 2200 eV to 2350 eV band where the two deepest M-IV and M-V edges are included. In the resultant reflectivity curves, we have clearly identified the fine structures associated with all the M-edges. Using these data, we calculated atomic scattering factor f1 as a function of X-ray energy, with which we have built the mirror response function which can be applied to the Suzaku spectra. As a result, we have found that discrepancy of the spectral model to the Suzaku data of 4U1630-472 (a black hole transient) and the Crab nebula around the M-edges are significantly reduced from those with the official Suzaku response.

ASTRO-H↗

On the Hunt for Detectable Biosignatures in Jezero Crater: What to Look for and Where

Introduction: The Perseverance rover, which is currently exploring Jezero crater on Mars, is equipped with seven instruments that allow for observation of textures, minerals, color, structure, and chemistry of rocks and sediments in order to search for signs of ancient life, understand the geologic history of the crater, and identify candidates for sample return (Farley et al. 2020). The first of these aims includes the direct detection of potential biosignatures, including textures, organic molecules, minerals, and elemental chemistries that are of biogenic origin (Mustard et al. 2013). The presence of these biosignatures will be constrained by the habitability of the local region, the preservation potential of the host rocks, and the sensitivity of the instrument suite, and their biogenicity will be investigated after return to Earth as part of the Mars Sample Return campaign. Here, we examine key targets on the three planned campaigns, potential biosignatures that may be present, and the capabilities of key rover instruments. High Potential Biosignature Sites in Jezero: To date, measurements have been made on multiple sites that both contain minerals known in terrestrial settings to preserve biosignatures and likely were habitable settings (Williford et al. 2021). Two examples include the fine-grained rocks at the base of the delta fan and the NW inner margin of the crater. Fine-grained Rocks at Base of Delta Fan. Fine-grained, clay-bearing rocks may have been deposited as muddy lake sediments that could have hosted life and preserved biosignatures settling out of the water column. The report of organic molecules by the Curiosity rover in the Sheepbed mudstone and Murray formation has highlighted this site in particular. Potential biosignatures in mudstones, especially those rich in silica (McMahon et al. 2018), microbialites and complex organics. NW Inner Margin of Crater. This unit, located along the inner margin of the crater, contains strong carbonate signatures and may have been the littoral zone of a lake (Horgan et al. 2020). The potential biosignatures here include microfossils, microbialites, biominerals, and complex organics. Detectability of Biosignatures by the Mars 2020 Instrument Suite: The Scanning Habitable Environments with Raman and Luminescence for Organics and Chemicals (SHERLOC) instrument comprises a Deep UV spectrometer, context imager, and color camera to generate spatially resolved chemical maps (Bhartia et al. 2020). It is sensitive to trace organics as well as a range of minerals and can detect native fluorescence from aromatic organics; the WATSON and ACI cameras can be used to observe morphologies such as stromatolitic laminations or filaments ranging from the tens of micron to millimeter scale. SHERLOC can detect organics that may be present in either of the high potential biosignature targets, as well as detect carbonates in the latter. However, the presence of high amounts of iron, such as in iron-rich clays, would cause attenuation of spectral response through UV absorption. The Planetary Instrument for X-ray Lithochemistry (PIXL) comprises an X-ray fluorescence spectrometer and camera that can scan rock surfaces to generate elemental maps (Allwood et al. 2020). PIXL can detect chemical biosignatures such as spatial variations of elemental abundances that may have resulted from biological activity. PIXL would be particularly useful in detecting fine textures and elemental chemistries in either high potential biosignature target, but cannot directly detect minerals such as carbonate. The SuperCam instrument performs three types of spectroscopy, color imaging, and acoustic recording to remotely examine elemental composition, minerals, organics, and textures (Maurice et al. 2021). Using laser induced breakdown spectroscopy and time resolved luminescence spectroscopy, SuperCam can detect major elemental building blocks of organics (i.e., C, H, N, O, P, S) and conjugated organic structures, respectively, which may be found in either site. While in other contexts, luminescence is a useful tool for biosignature identification, luminescence generated by the 532 nm laser may obscure the Raman signal. Conclusion: The three instruments discussed can be used collaboratively to establish the presence of potential biosignatures in samples. These high-priority samples may then be returned to Earth for detailed laboratory analysis.

S. Sharma↗

Spectroscopic and Geochemical Analyses of Ferrihydrite from Hydrothermal Springs in Iceland and Applications to Mars

Ferrihydrite samples were collected from a thermal spring and a cold stream in the Landmannalaugar region of Iceland. Chemical and spectroscopic analyses have been performed on the air-dried and fine-grained fractions of these samples. The ferrihydrite from the cold stream is a pure sample, containing small amounts of Ca, P and Si, which do not form minerals detectable with X-ray diffraction (XRD) or reflectance and transmittance spectroscopy. The ferrihydrite from the thermal pool is a less pure sample, containing larger amounts of amorphous Si and P. The XRD and spectral features for this sample are also consistent with a less crystalline structure. Some of the Si is incorporated in the structure of the ferrihydrite. The Ca, P and possibly some of the Si may be biogenic. The spectral character of these Icelandic ferrihydrites is compared with those of synthetic ferrihydrites and other iron oxide/oxyhydroxide minerals. Ferrihydrite is characterized by a broad Fe3+ excitation band near 0.92 microns (approx. 10900/cm) and a strong Fe-O absorption feature near 475/cm (approx. 21 microns) in transmittance spectra. Multiple bands due to H2O and OH are also present for ferrihydrite. Natural ferrihydrites frequently exhibit a band near 950-1050/cm (approx. 10 microns) that is typically not observed for synthetic ferrihydrites and may be due to some Si in the structure. An additional pair of spectral bands near 1400 and 1500/cm (approx. 7 microns) are characteristic of pure ferrihydrites from natural and synthetic sources. Hydrothermal springs may have been present at one time on Mars in association with volcanic activity. Ferrihydrite formation in such an environment may have contributed to the ferric oxide-rich surface material on Mars.

Bishop, Janice↗

Nature and origin of interstellar diamond from the Allende CV3 meteorite

Data and experimental evidence which support the contention that the C delta diamonds may result from grain-grain collisions in supernova shocks in the interstellar medium are presented. Fragments of the Allende CV3 chondrite were acid-treated. A whitish powder was obtained. For the Analytical Electron Microscopy (AEM) a small drop of ethanol suspension was transferred onto holey carbon support films on 3 mm EM grids. The AEM was performed on transmission-thin fragments of the material which overlay holes in the film, to eliminate interference from the substrate. Electron Spectroscopy for Chemical Analysis (ESCA) was performed on a large aliquot of C. Diamond was identified by selected area electron diffraction. Scanning Transmission Electron Microscope / Energy Dispersive X-ray (STEM-EDS) microanalyses of the C delta diamond, using a light-element detector, show that oxygen and possibly nitrogen are the only impurities consistently present. ESCA spectra from bulk C delta material confirm the presence of N at a level of 0.35 percent or less. Under UV irradiation a yellow-red fluorescence is observed, consistent with that of natural diamonds containing substitutional N. Electron Energy Loss Spectra (EELS) were recorded at 2 eV resolution from the C delta diamond, high pressure synthetic diamond, a diamond film produced in a low pressure plasma by chemical vapor deposition (CVD) on a heated silicon substrate (Roy, 1987), graphite, and amorphous arc sputtered carbon. Comparison of the carbon K edge shape and fine structure shows the Allende C delta phase to be largely diamond, but with a significant pre-edge absorption feature indicative of transitions of C 1s electrons into pi asterisk orbitals which are absent in the purely sp(3)-bonded diamond but present in graphite and amorphous carbon.

Blake, David↗

The Far-Infrared Emission Line and Continuum Spectrum of the Seyfert Galaxy NGC 1068

We report on the analysis of the first complete far-infrared spectrum (43-197 microns) of the Seyfert 2 galaxy NGC 1068 as observed with the Long Wavelength Spectrometer (LWS) onboard the Infrared Space Observatory (ISO). In addition to the 7 expected ionic fine structure emission lines, the OH rotational lines at 79, 119 and 163 microns were all detected in emission, which is unique among galaxies with full LWS spectra, where the 119 micron line, where detected, is always in absorption. The observed line intensities were modelled together with IS0 Short Wavelength Spectrometer (SWS) and optical and ultraviolet line intensities from the literature, considering two independent emission components: the AGN component and the starburst component in the circumnuclear ring of approximately 3kpc in size. Using the UV to mid-IR emission line spectrum to constrain the nuclear ionizing continuum, we have confirmed previous results: a canonical power-law ionizing spectrum is a poorer fit than one with a deep absorption trough, while the presence of a big blue bump is ruled out. Based on the instantaneous starburst age of 5 Myr constrained by the Br gamma equivalent width in the starburst ring, and starburst synthesis models of the mid- and far-infrared fine-structure line emission, a low ionization parameter (U=10(exp -3.5)) and low densities (n=100 cm (exp -3)) are derived. Combining the AGN and starburst components, we succeed in modeling the overall UV to far-IR atomic spectrum of SGC 1068, reproducing the line fluxes to within a factor 2.0 on average with a standard deviation of 1.4. The OH 119 micron emission indicates that the line is collisionally excited, and arises in a warm and dense region. The OH emission has been modeled using spherically symmetric, non-local, non-LTE radiative transfer models. The models indicate that the bulk of the emission arises from the nuclear region, although some extended contribution from the starburst is not ruled out. The OH abundance in the nuclear region is expected to be approximately 10(exp -5), characteristic of X-ray dominated regions.

Spinoglio, Luigi↗

X-Ray Microanalysis and Electron Energy Loss Spectrometry in the Analytical Electron Microscope: Review and Future Directions

This paper reviews and discusses future directions in analytical electron microscopy for microchemical analysis using X-ray and Electron Energy Loss Spectroscopy (EELS). The technique of X-ray microanalysis, using the ratio method and k(sub AB) factors, is outlined. The X-ray absorption correction is the major barrier to the objective of obtaining I% accuracy and precision in analysis. Spatial resolution and Minimum Detectability Limits (MDL) are considered with present limitations of spatial resolution in the 2 to 3 microns range and of MDL in the 0.1 to 0.2 wt. % range when a Field Emission Gun (FEG) system is used. Future directions of X-ray analysis include improvement in X-ray spatial resolution to the I to 2 microns range and MDL as low as 0.01 wt. %. With these improvements the detection of single atoms in the analysis volume will be possible. Other future improvements include the use of clean room techniques for thin specimen preparation, quantification available at the I% accuracy and precision level with light element analysis quantification available at better than the 10% accuracy and precision level, the incorporation of a compact wavelength dispersive spectrometer to improve X-ray spectral resolution, light element analysis and MDL, and instrument improvements including source stability, on-line probe current measurements, stage stability, and computerized stage control. The paper reviews the EELS technique, recognizing that it has been slow to develop and still remains firmly in research laboratories rather than in applications laboratories. Consideration of microanalysis with core-loss edges is given along with a discussion of the limitations such as specimen thickness. Spatial resolution and MDL are considered, recognizing that single atom detection is already possible. Plasmon loss analysis is discussed as well as fine structure analysis. New techniques for energy-loss imaging are also summarized. Future directions in the EELS technique will be the development of new spectrometers and improvements in thin specimen preparation. The microanalysis technique needs to be simplified and software developed so that the EELS technique approaches the relative simplicity of the X-ray technique. Finally, one can expect major improvements in EELS imaging as data storage and processing improvements occur.

Goldstein, J. I.↗