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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.

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At least 19 records
All sourcesNASA NTRSDOE OSTI
NASA NTRS1993

Microchemical analysis of the SCS-6 silicon carbide fiber

A detailed quantitative study of the microstructural variation of chemical composition of chemically vapor-deposited commercial SiC SCS-6 fiber is presented. Chemical etching and various electron-optical techniques including SEM, TEM, scanning Auger microscopy, AES, and parallel electron energy loss spectroscopy are used to analyze the chemical composition of the as-received fiber. In addition, some results on stereology of the high-temperature annealed fiber are presented. The results show that the carbon-to-silicon atom ratio in the SiC layers decreases in a stepwise fashion from about 3:2 to about 1:1 in going from the innermost layer to the outermost layer.

Ning, Xian-Jie↗
NASA NTRS1995

Microchemical Analysis Of Space Operation Debris

Report discusses techniques used in analyzing debris relative to space shuttle operations. Debris collected from space shuttle, expendable launch vehicles, payloads carried by space shuttle, and payloads carried by expendable launch vehicles. Optical microscopy, scanning electron microscopy with energy-dispersive spectrometry, analytical electron microscopy with wavelength-dispersive spectrometry, and X-ray diffraction chosen as techniques used in examining samples of debris.

Cummings, Virginia J.↗
NASA NTRS1996

Integrated Microchemical Analysis System Using DS2 Penetrator Technology for the Enantiomeric Detection of Amino Acids

Any strategy for investigating whether abiotic and/or biotic organic molecules are present on Mars and the search for biosignatures should focus on compounds which are readily synthesized under plausible prebiotic conditions, play an essential role in biochemistry as we know it and have properties such as chirality (handedness) which can be used to distinguish between abiotic vs. biotic origins (1). Amino acids are one of the few compound classes that fulfill all these requirements. They are synthesized in high yields in prebiotic simulation experiments, are one of the more abundant types of organic compounds present in carbonaceous meteorites and only the L-enantiomers are used in the proteins and enzymes in life on Earth.

Frank J Grunthaner↗
NASA NTRS1993

Procedures for analysis of debris relative to Space Shuttle systems

Debris samples collected from various Space Shuttle systems have been submitted to the Microchemical Analysis Branch. This investigation was initiated to develop optimal techniques for the analysis of debris. Optical microscopy provides information about the morphology and size of crystallites, particle sizes, amorphous phases, glass phases, and poorly crystallized materials. Scanning electron microscopy with energy dispersive spectrometry is utilized for information on surface morphology and qualitative elemental content of debris. Analytical electron microscopy with wavelength dispersive spectrometry provides information on the quantitative elemental content of debris.

Kim, Hae Soo↗
NASA NTRS2013

Atomic Force Microscope Mediated Chromatography

The atomic force microscope (AFM) is used to inject a sample, provide shear-driven liquid flow over a functionalized substrate, and detect separated components. This is demonstrated using lipophilic dyes and normal phase chromatography. A significant reduction in both size and separation time scales is achieved with a 25-micron-length column scale, and one-second separation times. The approach has general applications to trace chemical and microfluidic analysis. The AFM is now a common tool for ultra-microscopy and nanotechnology. It has also been demonstrated to provide a number of microfluidic functions necessary for miniaturized chromatography. These include injection of sub-femtoliter samples, fluidic switching, and sheardriven pumping. The AFM probe tip can be used to selectively remove surface layers for subsequent microchemical analysis using infrared and tip-enhanced Raman spectroscopy. With its ability to image individual atoms, the AFM is a remarkably sensitive detector that can be used to detect separated components. These diverse functional components of microfluidic manipulation have been combined in this work to demonstrate AFM mediated chromatography. AFM mediated chromatography uses channel-less, shear-driven pumping. This is demonstrated with a thin, aluminum oxide substrate and a non-polar solvent system to separate a mixture of lipophilic dyes. In conventional chromatographic terms, this is analogous to thin-layer chromatography using normal phase alumina substrate with sheardriven pumping provided by the AFM tip-cantilever mechanism. The AFM detection of separated components is accomplished by exploiting the variation in the localized friction of the separated components. The AFM tip-cantilever provides the mechanism for producing shear-induced flows and rapid pumping. Shear-driven chromatography (SDC) is a relatively new concept that overcomes the speed and miniaturization limitations of conventional liquid chromatography. SDC is based on a sliding plate system, consisting of two flat surfaces, one of which has a recessed channel. A fluid flow is produced by axially sliding one plate past another, where the fluid has mechanical shear forces imposed at each point along the channel length. The shear-induced flow rates are very reproducible, and do not have pressure or voltage gradient limitations. SDC opens up a new range of enhanced separation kinetics by permitting the sample confinement with submicron dimensions. Small, highly confined liquid is advantageous for chromatographic separation because the separation rate is known to scale according to the square of the confined sample diameter. In addition, because shear-driven flows are not limited by fluid velocity, shear-driven liquid chromatography may provide up to 100,000 plate efficiency.

Anderson, Mark S.↗
DOE OSTI2022

Stream and ocean hydrodynamics mediate partial migration strategies in an amphidromous Hawaiian goby

Abstract Partial migration strategies, in which some individuals migrate but others do not, are widely observed in populations of migratory animals. Such patterns could arise via variation in migratory behaviors made by individual animals, via genetic variation in migratory predisposition, or simply by variation in migration opportunities mediated by environmental conditions. Here we use spatiotemporal variation in partial migration across populations of an amphidromous Hawaiian goby to test whether stream or ocean conditions favor completing its life cycle entirely within freshwater streams rather than undergoing an oceanic larval migration. Across 35 watersheds, microchemical analysis of otoliths revealed that most adult Awaous stamineus were freshwater residents (62% of n = 316 in 2009, 83% of n = 274 in 2011), but we found considerable variation among watersheds. We then tested the hypothesis that the prevalence of freshwater residency increases with the stability of stream flows and decreases with the availability of dispersal pathways arising from ocean hydrodynamics. We found that streams with low variation of daily discharge were home to a higher incidence of freshwater residents in each survey year. The magnitude of the shift in freshwater residency between survey years was positively associated with predicted interannual variability in the success of larval settlement in streams on each island based on passive drift in ocean currents. We built on these findings by developing a theoretical model of goby life history to further evaluate whether mediation of migration outcomes by stream and ocean hydrodynamics could be sufficient to explain the range of partial migration frequency observed across populations. The model illustrates that the proportion of larvae entering the ocean and differential survival of freshwater‐resident versus ocean‐going larvae are plausible mechanisms for range‐wide shifts in migration strategies. Thus, we propose that hydrologic variation in both ocean and stream environments contributes to spatiotemporal variation in the prevalence of migration phenotypes in A. stamineus . Our empirical and theoretical results suggest that the capacity for partial migration could enhance the persistence of metapopulations of diadromous fish when confronted with variable ocean and stream conditions.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2023

Gas nitriding behavior of refractory metals and implications for multi-principal element alloy design

Multi-principal element alloys (MPEAs) comprise a large, flexible compositional space that enables tuning of their chemistry, structure, and properties. Here, to facilitate the development of nitriding-based surface-enhancement strategies that harness a broad compositional space, this study examined the gas nitriding behavior of Hf, Mo, Nb, Ta, Ti, and Zr as a function of time, temperature (750 and 1000 °C), and nitriding potential (i.e. ammonia-to-hydrogen ratio). These metals were selected because they have a strong driving force to form nitrides, and appear in many promising refractory MPEA compositions. The nitriding temperatures were selected based on the phase transformation temperature of Ti and Zr, and the nitriding potentials were chosen such that all elements are expected to form nitrides. Mass gain measurements indicate that all six elements follow parabolic kinetics. The microstructure observations and quantitative microchemical analysis show formation of dense and well-adhered compound layers for Mo, Nb, and Ta. Thick diffusion zones appear in Hf, Ta, Ti, and Zr, and diffusion coefficients were fit to the composition profiles. Partial delamination of the compound layer occurred for Ti and Zr. Peak hardness values above 30 GPa are obtained in the dense compound layers, and the solute hardening of the underlying alloy is correlated with the nitrogen content. The results provide insight into the dynamics of nitride compound formation relative to interstitial dissolution of nitrogen, and are discussed in the context of MPEA composition and processing design.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Final Technical Report. FG02-06ER54881

For over 25 years the Applied Superconductivity Center has been integral to the successful development of superconductors for magnetic confinement fusion reactors, culminating in being a part of the “dream team” assembled by the ITER Organization to address the failure of prototype ITER cable-in-conduit conductors to pass testing in the SULTAN facility, an issue that if not addressed successfully would have limited the useful lifetime of the reactor. While being called on through the years to address the immediate needs of facility construction we also continued fundamental studies of fusion applicable superconductors so that magnet designers could make use of improved performance, reliability and cost. The annual Low Temperature Superconductors workshops, jointly organized with LBNL, became the most important meeting for dissemination of data between university laboratories, national laboratories and industry.

2212↗
DOE OSTI2016

Report on Status of Shipment of High Fluence Austenitic Steel Samples for Characterization and Stress Corrosion Crack Testing

The goal of the Mechanisms of Irradiation Assisted Stress Corrosion Cracking (IASCC) task in the LWRS Program is to conduct experimental research into understanding how multiple variables influence the crack initiation and crack growth in materials subjected to stress under corrosive conditions. This includes understanding the influences of alloy composition, radiation condition, water chemistry and metallurgical starting condition (i.e., previous cold work or heat treatments and the resulting microstructure) has on the behavior of materials. Testing involves crack initiation and growth testing on irradiated specimens of single-variable alloys in simulated Light Water Reactor (LWR) environments, tensile testing, hardness testing, microstructural and microchemical analysis, and detailed efforts to characterize localized deformation. Combined, these single-variable experiments will provide mechanistic understanding that can be used to identify key operational variables to mitigate or control IASCC, optimize inspection and maintenance schedules to the most susceptible materials/locations, and, in the long-term, design IASCC-resistant materials. In support of this research, efforts are currently underway to arrange shipment of “free” high fluence austenitic alloys available through Électricité de France (EDF) for post irradiation testing at the Oak Ridge National Laboratory (ORNL) and IASCC testing at the University of Michigan. These high fluence materials range in damage values from 45 to 125 displacements per atom (dpa). The samples identified for transport to the United States, which include nine, no-cost, 304, 308 and 316 tensile bars, were relocated from the Research Institute of Atomic Reactors (RIAR) in Dimitrovgrad, Ulyanovsk Oblast, Russia, and received at the Halden Reactor in Halden, Norway, on August 23, 2016. ORNL has been notified that a significant amount of work is required to prepare the samples for further shipment to Oak Ridge, Tennessee. The preliminary work for sample shipment between Halden and Oak Ridge includes fabrication of an inner cask sample container, decontamination and preparation of a Type A container, preparation of new activity calculations, all necessary paperwork, and handling. ORNL will continue to work to track progress of sample preparation and shipment status, and to work toward an agreement that covers material shipping costs between the Halden Reactor and the Oak Ridge National Laboratory.

36 MATERIALS SCIENCE↗
NASA NTRS1992

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.↗
DOE OSTI2021

Phase Stability of Yttrium Titanium Oxide

This proposed study aims at elevating Idaho National Laboratory (INL)’s portfolio in nuclear material research on two major fronts: 1) expanding INL’s material characterization capabilities to provide holistic microstructural and microchemical characterization ranging from atomic scale to millimeter scale, and 2) filling the knowledge gap on the effect of microstructural evolution on material phase stability at extreme conditions resembling those inside nuclear reactors, using Yttrium-Titanium-Oxide (YTO) as a model material. Previous research indicated the kinetics of phase transition of YTO materials varies between bulk samples and powder samples, suggesting that microstructural characteristics such as defect, micro-strain, and crystallite size could play a significant role in phase transition. The effect of crystallite size on the thermodynamics of phase transition has been well documented for other ceramic materials at nanometer crystallite size, with potential impacts from surface and strain energy and defects. In this proposed study, we will perform microstructural (micro-strain, crystallite size, defects, phase) and microchemical (elemental mapping) analyses through in-situ high temperature measurements using X-ray diffraction (XRD; at millimeter scale for powder and bulk samples) and transmission electron microscopy (TEM, at nanometer scale and atomic scale for powder and thin foil samples), to provide a comprehensive view of the effect of microstructural and microchemical evolution on phase transition and phase stability of YTO materials. These findings will also establish a roadmap and provide new insights on the phase stability of other materials that are critical to nuclear energy and other renewable energy infrastructure. Besides advancing our understanding of this fundamental material science question, this project will also enable the development of state-of-the-art material characterization capabilities at INL/MFC for microstructural and microchemical analysis at high temperature conditions. The new collaboration between the High-Resolution Materials Characterization group at INL and the Electron Microscopy group at the University of Florida (UF) in this project will open the possibilities for more fruitful and synergetic cutting-edge nuclear material research in the future.

36 MATERIALS SCIENCE↗
NASA NTRS1993

Thermal Analyzer for Planetary Soil (TAPS): an in Situ Instrument for Mineral and Volatile-element Measurements

Thermal Analyzer for Planetary Soil (TAPS) offers a specific implementation for the generic thermal analyzer/evolved-gas analyzer (TA/EGA) function included in the Mars Environmental Survey (MESUR) strawman payload; applications to asteroids and comets are also possible. The baseline TAPS is a single-sample differential scanning calorimeter (DSC), backed by a capacitive-polymer humidity sensor, with an integrated sampling mechanism. After placement on a planetary surface, TAPS acquires 10-50 mg of soil or sediment and heats the sample from ambient temperature to 1000-1300 K. During heating, DSC data are taken for the solid and evolved gases are swept past the water sensor. Through ground based data analysis, multicomponent DSC data are deconvolved and correlated with the water release profile to quantitatively determine the types and relative proportions of volatile-bearing minerals such as clays and other hydrates, carbonates, and nitrates. The rapid-response humidity sensors also achieve quantitative analysis of total water. After conclusion of soil-analysis operations, the humidity sensors become available for meteorology. The baseline design fits within a circular-cylindrical volume less than 1000 cm(sup 3), occupies 1.2 kg mass, and consumes about 2 Whr of power per analysis. Enhanced designs would acquire and analyze multiple samples and employ additional microchemical sensors for analysis of CO2, SO2, NO(x), and other gaseous species. Atmospheric pumps are also being considered as alternatives to pressurized purge gas.

Gooding, J. L.↗
NASA NTRS2014

Nanoscale Analysis of Space-Weathering Features in Soils from Itokawa

Space weathering alters the spectral properties of airless body surface materials by redden-ing and darkening their spectra and attenuating characteristic absorption bands, making it challenging to characterize them remotely [1,2]. It also causes a discrepency between laboratory analysis of meteorites and remotely sensed spectra from asteroids, making it difficult to associate meteorites with their parent bodies. The mechanisms driving space weathering include mi-crometeorite impacts and the interaction of surface materials with solar energetic ions, particularly the solar wind. These processes continuously alter the microchemical and structural characteristics of exposed grains on airless bodies. The change of these properties is caused predominantly by the vapor deposition of reduced Fe and FeS nanoparticles (npFe(sup 0) and npFeS respectively) onto the rims of surface grains [3]. Sample-based analysis of space weathering has tra-ditionally been limited to lunar soils and select asteroidal and lunar regolith breccias [3-5]. With the return of samples from the Hayabusa mission to asteroid Itoka-wa [6], for the first time we are able to compare space-weathering features on returned surface soils from a known asteroidal body. Analysis of these samples will contribute to a more comprehensive model for how space weathering varies across the inner solar system. Here we report detailed microchemical and microstructal analysis of surface grains from Itokawa.

Thompson, M. S.↗