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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 811 records · Page 45
All sourcesNASA NTRSDOE OSTI
DOE OSTI2022

Impacts of Crystalline Host Rock on Repository Barrier Materials at 250 °C: Hydrothermal Co-Alteration of Wyoming Bentonite and Steel in the Presence of Grimsel Granodiorite

Direct disposal of dual-purpose canisters (DPC) has been proposed to streamline the disposal of spent nuclear fuel. However, there are scenarios where direct disposal of DPCs may result in temperatures in excess of the specified upper temperature limits for some engineered barrier system (EBS) materials, which may cause alteration within EBS materials dependent on local conditions such as host rock composition, chemistry of the saturating groundwaters, and interactions between barrier materials themselves. Here we report the results of hydrothermal experiments reacting EBS materials—bentonite buffer and steel—with an analogue crystalline host rock and groundwater at 250 °C. Experiment series explored the effect of reaction time on the final products and the effects of the mineral and fluid reactants on different steel types. Post-mortem X-ray diffraction, electron microprobe, and scanning electron microscopy analyses showed characteristic alteration of both bentonite and steel, including the formation of secondary zeolite and calcium silicate hydrate minerals within the bentonite matrix and the formation of iron-bearing clays and metal oxides at the steel surfaces. Swelling clays in the bentonite matrix were not quantitatively altered to non-swelling clay species by the hydrothermal conditions. The combined results of the solution chemistry over time and post-mortem mineralogy suggest that EBS alteration is more sensitive to initial groundwater chemistry than the presence of host rock, where limited potassium concentration in the solution prohibits conversion of the smectite minerals in the bentonite matrix to non-swelling clay species.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2023

Understanding of Active Sites and Interconversion of Pd and PdO during CH 4 Oxidation

Pd-based catalysts are widely used in the oxidation of CH 4 and have a significant impact on global warming. However, understanding their active sites remains controversial, because interconversion between Pd and PdO occurs consecutively during the reaction. Understanding the intrinsic active sites under reaction conditions is critical for developing highly active and selective catalysts. In this study, we demonstrated that partially oxidized palladium (PdO x ) on the surface plays an important role for CH 4 oxidation. Regardless of whether the initial state of Pd corresponds to oxides or metallic clusters, the topmost surface is PdO x , which is formed during CH4 oxidation. A quantitative analysis using CO titration, diffuse reflectance infrared Fourier-transform spectroscopy, X-ray diffraction, and scanning transmission electron microscopy demonstrated that a surface PdO layer was formed on top of the metallic Pd clusters during the CH 4 oxidation reaction. Furthermore, the time-on-stream test of CH 4 oxidation revealed that the presence of the PdO layer on top of the metallic Pd clusters improves the catalytic activity. Our periodic density functional theory (DFT) calculations with a PdO x slab and nanoparticle models aided the elucidation of the structure of the experimental PdO particles, as well as the experimental C-O bands. The DFT results also revealed the formation of a PdO layer on the metallic Pd clusters. This study helps achieve a fundamental understanding of the active sites of Pd and PdO for CH 4 oxidation and provides insights into the development of active and durable Pd-based catalysts through molecular-level design.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2020

Styrene-Based Elastomer Composites with Functionalized Graphene Oxide and Silica Nanofiber Fillers: Mechanical and Thermal Conductivity Properties

The mechanical and thermal conductivity properties of two composite elastomers were studied. Styrene–butadiene rubber (SBR) filled with functionalized graphene oxide (GO) and silica nanofibers, and styrene–butadiene–styrene (SBS) block copolymers filled with graphene oxide. For the SBR composites, GO fillers with two different surface functionalities were synthesized (cysteamine and dodecylamine) and dispersed in the SBR using mechanical and liquid mixing techniques. The hydrophilic cysteamine-based GO fillers were dispersed in the SBR by mechanical mixing, whereas the hydrophobic dodecylamine-based GO fillers were dispersed in the SBR by liquid mixing. Silica nanofibers (SnFs) were fabricated by electrospinning a sol–gel precursor solution. The surface chemistry of the functionalized fillers was studied in detail. The properties of the composites and the synergistic improvements between the GO and SnFs are presented. For the SBS composites, GO fillers were dispersed in the SBS elastomer at several weight percent loadings using liquid mixing. Characterization of the filler material and the composite elastomers was performed using x-ray photoelectron spectroscopy, x-ray diffraction, transmission electron microscopy, scanning electron microscopy, thermogravimetric analysis, dynamic mechanical analysis, tensile testing, nanoindentation, thermal conductivity and abrasion testing.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Synthesis of epitaxial TaO$_2$ thin films on Al$_2$O$_3$ by suboxide molecular-beam epitaxy and thermal laser epitaxy

Tantalum dioxide (TaO2) is a metastable tantalum compound. Here, we report the epitaxial stabilization of TaO2 on Al2O3 (1-102) (r-plane sapphire) substrates using suboxide molecular-beam epitaxy (MBE) and thermal laser epitaxy (TLE), demonstrating single-oriented, monodomain growth of anisotropically strained thin films. Microstructural investigation is performed using synchrotron X-ray diffraction and scanning transmission electron microscopy. The tetravalent oxidation state of tantalum is confirmed using X-ray absorption and photoemission spectroscopy as well as electron energy-loss spectroscopy. Optical properties are investigated via spectroscopic ellipsometry and reveal a 0.3 eV Mott gap of the tantalum 5d electrons. Density-functional theory and group theoretical arguments are used to evaluate the limited stability of the rutile phase and reveal the potential to unlock a hidden metal-insulator transition concomitant with a structural phase transition to a distorted rutile phase, akin to NbO2. Our work expands the understanding of tantalum oxides and paves the way for their integration into next-generation electronic and photonic devices.

FOS: Physical sciences↗
DOE OSTI2022

Exposure of Stainless Steel 316 to Subcritical, Transition, and Near-Supercritical Water

This work investigates the oxidation of austenitic stainless steel 316 at temperatures close to the critical point of water: subcritical water at 330°C and 27 MPa, the transition between subcritical and supercritical water at 374°C and 27 MPa, and supercritical water (SCW) at 380°C and 27 MPa. The surfaces of the samples were characterized using x-ray diffraction, Raman spectroscopy, scanning electron microscopy, and x-ray photoelectron spectroscopy before and after exposure. Magnetite (Fe3O4) was found to be present on all surfaces of all samples. The samples exposed to subcritical water also showed the presence of a nickel-iron chromium mixed spinel Ni(Fe2-xCrx)O4. The oxide morphology was observed to vary based on exposure temperature; an increased nucleation and growth rate, and an increased generation of Fe2+ was observed on samples exposed to the transition region and SCW.

Materials Science↗
NASA NTRS1973

Investigation of KC-135 flight samples solidified in near-zero gravity

An analysis was conducted of three KC-135 flight samples that had been solidified in near-zero gravity. These samples had been generated during near-zero gravity testing of M553 experiment Skylab flight hardware. The samples evaluated were all Star-J Satellite, a cobalt base alloy. The analytical procedures (optical microscopy, scanning electron microscopy, electron microprobe, X-ray diffraction, differential scanning calorimetry, and microhardness) to be use on the Skylab flight samples were optimized and the analytical results are presented.

Larson, D., Jr.↗
NASA NTRS1988

Crystallization kinetics of BaO-Al2O3-SiO2 glasses

Barium aluminosilicate glasses are being investigated as matrix materials in high-temperature ceramic composites for structural applications. Kinetics of crystallization of two refractory glass compositions in the barium aluminosilicate system were studied by differential thermal analysis (DTA), X-ray diffraction (XRD), and scanning electron microscopy (SEM). From variable heating rate DTA, the crystallization activation energies for glass compositions (wt percent) 10BaO-38Al2O3-51SiO2-1MoO3 (glass A) and 39BaO-25Al2O3-35SiO2-1MoO3 (glass B) were determined to be 553 and 558 kJ/mol, respectively. On thermal treatment, the crystalline phases in glasses A and B were identified as mullite (3Al2O3-2SiO2) and hexacelsian (BaO-Al2O3-2SiO2), respectively. Hexacelsian is a high-temperature polymorph which is metastable below 1590 C. It undergoes structural transformation into the orthorhombic form at approximately 300 C accompanied by a large volume change which is undesirable for structural applications. A process needs to be developed where stable monoclinic celsian, rather than hexacelsian, precipitates out as the crystal phase in glass B.

Bansal, Narottam P.↗
NASA NTRS1989

Crystallization kinetics of BaO-Al2O3-SiO2 glasses

Barium aluminosilicate glasses are being investigated as matrix materials in high-temperature ceramic composites for structural applications. Kinetics of crystallization of two refractory glass compositions in the barium aluminosilicate system were studied by differential thermal analysis (DTA), X-ray diffraction (XRD), and scanning electron microscopy (SEM). From variable heating rate DTA, the crystallization activation energies for glass compositions (wt percent) 10BaO-38Al2O3-51SiO2-1MoO3 (glass A) and 39BaO-25Al2O3-35SiO2-1MoO3 (glass B) were determined to be 553 and 558 kJ/mol, respectively. On thermal treatment, the crystalline phases in glasses A and B were identified as mullite (3Al2O3-2SiO2) and hexacelsian (BaO-Al2O3-2SiO2), respectively. Hexacelsian is a high-temperature polymorph which is metastable below 1590 C. It undergoes structural transformation into the orthorhombic form at approximately 300 C accompanied by a large volume change which is undesirable for structural applications. A process needs to be developed where stable monoclinic celsian, rather than hexacelsian, precipitates out as the crystal phase in glass B.

Bansal, Narottam P.↗
NASA NTRS1988

Growth and characterization of CdTe on GaAs/Si substrates

Epitaxial CdTe has been grown on both (100) GaAs/Si and (111) GaAs/Si substrates. A combination of molecular beam epitaxy and metal organic chemical vapor deposition have been employed to achieve this growth. The GaAs layers are grown in Si substrates by molecular beam epitaxy, followed by the growth of CdTe on GaAs/Si substra by metalorganic chemical vapor deposition. X-ray diffraction, photoluminescence, and scanning electron microscopy have been used to characterize the CdTe films.

Radhakrishnan, G.↗
NASA NTRS1994

Quantitative reflectance spectroscopy of buddingtonite from the Cuprite mining district, Nevada

Buddingtonite, an ammonium-bearing feldspar diagnostic of volcanic-hosted alteration, can be identified and, in some cases, quantitatively measured using short-wave infrared (SWIR) reflectance spectroscopy. In this study over 200 samples from Cuprite, Nevada, were evaluated by X ray diffraction, chemical analysis, scanning electron microscopy, and SWIR reflectance spectroscopy with the objective of developing a quantitative remote-sensing technique for rapid determination of the amount of ammonium or buddingtonite present, and its distribution across the site. Based upon the Hapke theory of radiative transfer from particulate surfaces, spectra from quantitative, physical mixtures were compared with computed mixture spectra. We hypothesized that the concentration of ammonium in each sample is related to the size and shape of the ammonium absorption bands and tested this hypothesis for samples of relatively pure buddingtonite. We found that the band depth of the 2.12-micron NH4 feature is linearly related to the NH4 concentration for the Cuprite buddingtonite, and that the relationship is approximately exponential for a larger range of NH4 concentrations. Associated minerals such as smectite and jarosite suppress the depth of the 2.12-micron NH4 absorption band. Quantitative reflectance spectroscopy is possible when the effects of these associated minerals are also considered.

Felzer, Benjamin↗
NASA NTRS2001

Crystallographic Texture and Orientation Variants in Al2O3-Y3Al5O12 Directionally Solidified Eutectic Crystals

Eutectic rods of Al2O3 and Y3Al5O12 were grown by a laser-heated float zone method, and their microstructure and crystallographic texture were studied by scanning electron microscopy, electron backscattered diffraction and x-ray diffraction. The composites were found to be highly textured with two twin-related crystallographic orientation relationships between the phases. Electron backscattered diffraction was employed to determine the spatial distribution of the orientational variants within the samples and to define the crystallographic orientation of various microstructural features.

Frazer, Colleen S.↗
NASA NTRS2003

Oxidation of ZrB2-and HfB2-Based Ultra-High Temperature Ceramics: Effects of Ta Additions

Several compositions of ZrB2- and HfB2-based Ultra-High Temperature Ceramics (UHTC) were oxidized in stagnant air at 1627 C in ten minute cycles for times up to 100 minutes. These compositions include: ZrB2 - 20v% SiC, HfB2 - 20v% SiC, ZrB2 - 20v% SiC - 20v% TaSi2, ZrB2 - 33v% SiC, HfB2 - 20v% SiC - 20v% TaSi2, and ZrB2 - 20v% SiC - 20v% TaC. The weight change due to oxidation was recorded. The ZrB2 - 20v% SiC - 20v% TaSi2 composition was also oxidized in stagnant air at 1927 C and in an arc jet atmosphere. Samples were analyzed after oxidation by x-ray diffraction, field emission scanning electron microscopy, and energy dispersive spectroscopy to determine the reaction products and to observe the microstructure. The ZrB2 - 20v% SiC - 20v% TaSi2 showed the lowest oxidation rate at 1627 C, but performed poorly under the more extreme tests due to liquid phase formation. Effects of Ta-additions on the oxidation of the diboride-based UHTC are discussed.

Opila, Elizabeth↗
NASA NTRS2004

Oxidation of High-temperature Alloy Wires in Dry Oxygen and Water Vapor

Small diameter wires (150 to 250 microns) of the high temperature alloys Haynes 188, Haynes 230, Haynes 230, Haynes 214, Kanthal Al and PM2000 were oxidized at 1204 C in dry oxygen or 50% H2O /50% O2 for 70 Hours. The oxidation kinetics were monitored using a thermogravimetric technique. Oxide phase composition and morphology of the oxidized wires were determined by X-ray diffraction,field emission scanning electron microscopy, and energy dispersive spectroscopy. The alumina-forming alloys, Kanthal Al and PM2000, out-performed the chromia-forming alloys under this conditions. PM2000 was recommended as the most promising candidate for advanced hybrid seal applications for space reentry control surface seals or hypersonic propulsion system seals. This study also demonstrated that thermogravimetric analysis of small diameter wires is a powerful technique for the study of oxide volatility, oxide adherence, and breakaway oxidation.

Opila, Elizabeth J.↗
NASA NTRS2014

Pu'u Poli'ahu, Mauna Kea: A Possible Analog for the Hematite Bearing Layer Located in Gale Crater, Mars.

Hyperspectral data detected by the Compact Reconnaissance Imaging Spectrometer for Mars (CRISM) on board Mars Reconnaissance Orbiter (MRO) indicated the presence of a hematite bearing ridge on Mount Sharp situated in the Gale Crater, Mars. [Fraeman]. The presence of this mineral in high concentrations is indicative of possible aqueous origins. [Fraeman] In 2012, Curiosity Rover landed in Gale Crater on Mars. Curiosity's mission is to determine Mars' habitability and is equipped with an advanced suite of scientific instruments that are capable of conducting analyses on rocks and soil. The hematite bearing ridge on Mount Sharp is thought to be a good candidate of study for Curiosity. To better understand this type of terrain, the study of analog sites similar in geologic setting is of great importance. One site thought to be a comparable analog is a cinder cone called Pu'u Poli'ahu located on the summit of Mauna Kea, Hawaiʻi. Poli'ahu is unique among the tephra cones of Mauna Kea because it is thought to have formed in subaqueous conditions approximately 170,000 to 175,000 years ago. [Porter] Consequently located on the inner flanks of Poli'ahu is a rock outcrop that contains hematite. Samples were collected from the outcrop and characterized using the following instruments: Digital Microscope, Panalytical X‐ray diffraction (XRD), and scanning electron microscope (SEM). The initial preparation of the rocks involved documenting each sample by creating powdered samples, thick sections, and photo documentation.

Adams, M. E.↗
NASA NTRSDate not supplied

Habitability Potential of Martian Hydrothermal Systems Constrained from Exploration of a Magma-Sediment Hydrothermal System in the Colorado Plateau

Mars has a crust predominately composed of basalt, which displays wide-spread processes including volcanic hydrothermal systems and reference within. There is an abundance of evidence of previous low temperature hydrous alteration; however, finding evidence of high-temperature hydrothermal activity has been challenging. Therefore, we are investigating a mafic dike and the surrounding metamorphic contact zone to constrain how to find such systems on Mars and their habitability potential on Earth and by extension Mars. DC Dike (DCD) is in the Colorado Plateau, in south-central Utah, and intruded the Entrada formation Sandstone between 3.8 and 4.6 Ma. We chose Mars analog instrumentation to make our results directly applicable to those on Mars: Visible-Near Infrared reflectance spectroscopy (VNIR), X-Ray Diffraction (XRD), and Scanning Electron Microscope (SEM). 21 samples were analyzed with an Ore Express VNIR with wavelengths from 350-2500 nm. Bulk mineralogy is determined by using a Panalytical XRD including for clay fraction and soil separation analysis. Finally, samples are prepped as thin sections and will be analyzed using a SEM. All these techniques will be used to constrain: the mineralogy of the system, how the hydrothermal system cooled, the habitability of the cooling system, and how DCD relates to similar dikes in the area and on Mars. All of these results will then be compared to similar systems Mars, and if they too could have been habitable environments.

R. A. Slank↗
DOE OSTI2016

Three-Dimensional FIB/EBSD Characterization of Irradiated HfAl3-Al Composite

A thermal neutron absorbing material, comprised of 28.4 vol% HfAl3 in an Al matrix, was developed to serve as a conductively cooled thermal neutron filter to enable fast flux materials and fuels testing in a pressurized water reactor. In order to observe the microstructural change of the HfAl3-Al composite due to neutron irradiation, an EBSD-FIB characterization approach is developed and presented in this paper. Using the focused ion beam (FIB), the sample was fabricated to 25µm × 25µm × 20 µm and mounted on the grid. A series of operations were carried out repetitively on the sample top surface to prepare it for scanning electron microscopy (SEM). First, a ~100-nm layer was removed by high voltage FIB milling. Then, several cleaning passes were performed on the newly exposed surface using low voltage FIB milling to improve the SEM image quality. Last, the surface was scanned by Electron Backscattering Diffraction (EBSD) to obtain the two-dimensional image. After 50 to 100 two-dimensional images were collected, the images were stacked to reconstruct a three-dimensional model using DREAM.3D software. Two such reconstructed three-dimensional models were obtained from samples of the original and post-irradiation HfAl3-Al composite respectively, from which the most significant microstructural change caused by neutron irradiation apparently is the size reduction of both HfAl3 and Al grains. The possible reason is the thermal expansion and related thermal strain from the thermal neutron absorption. This technique can be applied to three-dimensional microstructure characterization of irradiated materials.

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗
DOE OSTI2019

Improved Crystalline Structure and Enhanced Photoluminescence of ZnO Nanolayers in B i2 Se 3 /ZnO Heterostructures

The Bi 2 Se 3 /ZnO heterostructure is a new combination of high- and low-band-gap nanomaterials that can be implemented for optoelectronic devices. The influence of the Bi 2 Se 3 substrate on crystallization of ZnO nanolayers and charge separation at the Bi 2 Se 3 /ZnO interface reflects these important parameters, which affect optical and electronic properties of the heterostructure. Despite a few studies on Bi 2 Se 3 /ZnO heterostructures, the mechanisms of enhanced optical properties and correlation between optical and structural properties in such heterostructures are not studied in detail. In the present paper, we report on structure and optical properties of ZnO nanolayers with different thicknesses (10–150 nm) deposited by atomic layer deposition on planar and nonplanar Bi 2 Se 3 nanostructured coatings. Crystallization of ZnO nanolayers grown on Bi 2 Se 3 and Si substrates was analyzed by X-ray diffraction and scanning and transmission electron microscopy methods. Enhancement of ZnO photoluminescence in Bi 2 Se 3 /ZnO heterostructures in comparison to the photoluminescence of ZnO nanolayers of the same thickness deposited on p-doped Si substrates was observed. Correlation between the structure and optical properties of ZnO nanolayers in Bi 2 Se 3 /ZnO heterostructures is analyzed. Three complementary mechanisms of enhancement of optical properties of ZnO in Bi 2 Se 3 /ZnO heterostructures, based on charge separation at the Bi 2 Se 3 /ZnO interface, improvement of ZnO crystalline structure, and surface-plasmon–photon coupling, are proposed. The Bi 2 Se 3 /ZnO heterostructure is a new combination of high- and low-band-gap nanomaterials that can be implemented for optoelectronic devices. The influence of the Bi 2 Se 3 substrate on crystallization of ZnO nanolayers and charge separation at the Bi 2 Se 3 /ZnO interface reflects these important parameters, which affect optical and electronic properties of the heterostructure. Despite a few studies on Bi 2 Se 3 /ZnO heterostructures, the mechanisms of enhanced optical properties and correlation between optical and structural properties in such heterostructures are not studied in detail. In the present paper, we report on structure and optical properties of ZnO nanolayers with different thicknesses (10–150 nm) deposited by atomic layer deposition on planar and nonplanar Bi 2 Se 3 nanostructured coatings. Crystallization of ZnO nanolayers grown on Bi 2 Se 3 and Si substrates was analyzed by X-ray diffraction and scanning and transmission electron microscopy methods. Enhancement of ZnO photoluminescence in Bi 2 Se 3 /ZnO heterostructures in comparison to the photoluminescence of ZnO nanolayers of the same thickness deposited on p-doped Si substrates was observed. Correlation between the structure and optical properties of ZnO nanolayers in Bi 2 Se 3 /ZnO heterostructures is analyzed. Finally, three complementary mechanisms of enhancement of optical properties of ZnO in Bi 2 Se 3 /ZnO heterostructures, based on charge separation at the Bi 2 Se 3 /ZnO interface, improvement of ZnO crystalline structure, and surface-plasmon–photon coupling, are proposed.

36 MATERIALS SCIENCE↗
DOE OSTI2023

High Thermoelectric Performance in 2D Sb 2 Te 3 and Bi 2 Te 3 Nanoplate Composites Enabled by Energy Carrier Filtering and Low Thermal Conductivity

Thermoelectrics are an important class of materials with great potential in alternative energy applications. In this study, two-dimensional (2D) nanoplates of the layered chalcogenides, Sb 2 Te 3 and Bi 2 Te 3 , are synthesized and composites of the two are investigated for their thermoelectric properties. The two materials, Sb 2 Te 3 and Bi 2 Te 3 , were synthesized as hexagonal, 2D nanoplates via a colloidal polyol route. The as-synthesized Sb 2 Te 3 and Bi 2 Te 3 vary drastically from one another in their lateral and vertical dimensions as revealed by scanning electron microscopy and atomic force microscopy. The single crystalline nanoplate nature is deduced by high-resolution transmission electron microscopy and selected area electron diffraction. Nanoplates have well-defined hexagonal facets as seen in the scanning and transmission electron microscopy images. The nanoplates were consolidated as an anisotropic nanostructured pellet via spark plasma sintering. Preferred orientation observed in the powder X-ray diffraction pattern and scanning electron microscopy images of the fractured pellets confirm the anisotropic structure of the nanoplates. Thermoelectric properties in the parallel and perpendicular directions were measured, revealing strong anisotropy with a significant reduction to thermal conductivity in the perpendicular direction due to increased phonon scattering at nanoplate interfaces. All compositions, except that of the 25% Bi 2 Te 3 nanoplate composite, behave as degenerate semiconductors with increasing electrical resistivity as the temperature increases. The Seebeck coefficient is also increased dramatically in the nanocomposites, the highest reaching 210 μV/K for 15% Bi 2 Te 3 . The increase in Seebeck is attributed to energy carrier filtering at the nanoplate interfaces. Overall, these enhanced thermoelectric properties lead to a drastic increase in the thermoelectric performance in the perpendicular direction, with zT ~ 1.26, for the 15% Bi 2 Te 3 nanoplate composite at 450 K.

36 MATERIALS SCIENCE↗