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At least 865 records · Page 48
All sourcesNASA NTRSDOE OSTI
NASA NTRS2000

Directionally Solidified Ceramics Produced

Produced Multiphase, interpenetrating structures are an alternative route to obtaining structural ceramic materials with adequate strength, toughness, and stability for high-temperature aerospace applications. The eutectic architecture, a continuous-reinforcing phase within a higher volume phase or matrix, can be described as a naturally occurring, in situ composite. The phases of a eutectic are thermodynamically compatible at high homologous temperatures. Strong and stable materials have been produced. Toughness, however, remains a technical obstacle. The potential for producing materials with enhanced toughness along with adequate strength and stability was demonstrated using the laser-heated float zone (LHFZ) growth method at the NASA Glenn Research Center at Lewis Field. LHFZ growth at Glenn provides a means to efficiently produce and record the underlying growth phenomena associated with two-phase structures. To initiate directional solidification, a seed of single-crystal sapphire (<0001> direction) was lowered onto the molten liquid until wetting occurred and then withdrawn at a constant rate. Neither the crystal nor the source rod was rotated. The materials produced were tested mechanically in tension, and the resulting microstructure was examined with a scanning electron microscope. Both the inherent properties of the constituent phases and the properties of the interface between them affect the mechanical behavior and the fracture surfaces. The following scanning electron micrographs show the microstructures of two different materials that were tested to failure in tension. In the left micrograph, the flat fracture surface is typical of a material that is strong but has low toughness. In the right micrograph, the crack is effectively deflected at the interface between the two phases, achieving higher toughness at moderately lower strength levels. Conducting mechanical tests to determine the high temperature properties of these materials is the next step in determining their eventual suitability.

Farmer, Serene C.↗
NASA NTRS2001

Coarsening Experiment Being Prepared for Flight

The Coarsening in Solid-Liquid Mixtures-2 (CSLM-2) experiment is a materials science space flight experiment whose purpose is to investigate the kinetics of competitive particle growth within a liquid matrix. During coarsening, small particles shrink by losing atoms to larger particles, causing the larger particles to grow. In this experiment, solid particles of tin will grow (coarsen) within a liquid lead-tin eutectic matrix. The preceding figures show the coarsening of tin particles in a lead-tin eutectic as a function of time. By conducting this experiment in a microgravity environment, we can study a greater range of solid volume fractions, and the effects of sedimentation present in terrestrial experiments will be negligible. The CSLM-2 experiment is slated to fly onboard the International Space Station. The experiment will be run in the Microgravity Science Glovebox installed in the U.S. Laboratory module.

Hickman, J. Mark↗
NASA NTRS2005

Wear of Selected Oxide Ceramics and Coatings

The use of oxide ceramics and coatings for moving mechanical components operating in high-temperature, oxidizing environments creates a need to define the tribological performance and durability of these materials. Results of research focusing on the wear behavior and properties of Al2O3/ZrO2 (Y2O3) eutectics and coatings under dry sliding conditions are discussed. The importance of microstructure and composition on wear properties of directionally solidified oxide eutectics is illustrated. Wear data of selected oxide-, nitride-, and carbide-based ceramics and coatings are given for temperatures up to 973K in air.

Miyoshi, K.↗
NASA NTRS2003

Coarsening Experiment Prepared for Flight

The Coarsening in Solid-Liquid Mixtures-2 (CSLM-2) experiment is a materials science spaceflight experiment whose purpose is to investigate the kinetics of competitive particle growth within a liquid matrix. During coarsening, small particles shrink by losing atoms to larger particles, causing the larger particles to grow. In this experiment, solid particles of tin will grow (coarsen) within a liquid lead-tin eutectic matrix. The following figures show the coarsening of tin particles in a lead-tin (Pb-Sn) eutectic as a function of time. By conducting this experiment in a microgravity environment, we can study a greater range of solid volume fractions, and the effects of sedimentation present in terrestrial experiments will be negligible. The CSLM-2 experiment flew November 2002 on space shuttle flight STS-113 for operation on the International Space Station, but it could not be run because of problems with the Microgravity Science Glovebox in the U.S. Laboratory module. Additional samples will be sent to ISS on subsequent shuttle flights.

Hickman, J. Mark↗
NASA NTRS2006

Silica and Pyroxene in IVA Irons; Possible Formation of the IVA Magma by Impact Melting and Reduction of L-LL-Chondrite Materials Followed by Crystallization and Cooling

Group IVA is a large magmatic group of iron meteorites. The mean DELTA O-17 (= delta O-17 - 0.52(raised dot) delta O-18) of the silicates is approx. plus or minus 1.2%o, similar to the highest values in L chondrites and the lowest values in LL chondrites; delta O-18 values are also in the L/LL range. This strongly suggests that IVA irons formed by melting L-LL parental material, but the mean Ni content of IVA irons (83 mg/g) is much lower than that of a presumed L-LL parent (approx. 170 mg/g) and the low-Ca pyroxene present in two IVA meteorites is Fs13, much lower than the Fs20-29 values in L and LL chondrites. Thus, formation from L-LL precursors requires extensive addition of metallic Fe, probably produced by reduction of FeS and FeO. Group IVA also has S/Ni, Ga/Ni, and Ge/Ni ratios that are much lower than those in L-LL chondrites or any chondrite group that preserves nebular compositions, implying loss of these volatile elements during asteroidal processing. We suggest that these reduction and loss processes occurred near the surface of the asteroid during impact heating, and resulted partly from reduction by C, and partly from the thermal dissociation of FeS and FeO with loss of O and S. The hot (approx. 1770 K) low-viscosity melt quickly moved through channels in the porous asteroid to form a core. Two members of the IVA group, Sao Joao Nepomuceno (hereafter, SJN) and Steinbach, contain moderate amounts of orthopyroxene and silica, and minor amounts of low-Ca clinopyroxene. Even though SJN formed after approx. 26% crystallization and Steinbach formed after approx. 77% Crystallization of the IVA core, both could have originated within several tens of meters of the core-mantle interface if 99% of the crystallization occurred from the center outwards. Two other members of the group (Gibeon and Bishop Canyon) contain tabular tridymite, which we infer to have initially formed as veins deposited from a cooling SiO-rich vapor. The silicates were clearly introduced into IVA irons after the initial magma crystallized. Because the y-iron crystals in SJN are typically about 5 cm across, an order of magnitude smaller than in IVA irons that do not contain massive silicates, we infer that the metal was in the gamma-iron field when the silicates were injected. The SJN and Steinbach silicate compositions are near the low-Ca-pyroxene/silica eutectic compositions. We suggest that a tectonic event produced a eutectic-like liquid and injected it together with unmelted pyroxene grains into fissures in the solid metal core. Published estimates of IVA metallographic cooling rates range from 20 to 3000 K/Ma, leading to a hypothesized breakup of the core during a major impact followed by scrambling of the core and mantle debris [Haack, H., Scott, E.R.D., Love, S.G., Brearley, A. 1996. Thermal histories of IVA stony-iron and iron meteorites: evidence for asteroid fragmentation and reaccretion. Geochim. Cosmochim. Acta 60, 3103-3113]. This scrambling model is physically implausible and cannot explain the strong correlation of estimated cooling rates with metal composition. Previous workers concluded that the low-Ca clinopyroxene in SJN and Steinbach formed from protopyroxene by quenching at a cooling rate of 10(sup 12) K/Ma, and suggested that this also supported an impact-scrambling model. This implausible spike in cooling rate by a factor of 10(sup 10) can be avoided if the low-Ca clinopyroxene were formed by a late shock event that converted orthopyroxene to clinopyroxene followed by minimal growth in the clinopyroxene field, probably because melt was also produced. We suggest that metallographic cooling-rate estimates (e.g., based on island taenite) giving similar values throughout the metal compositional range are more plausible, and that the IVA parent asteroid can be modeled by monotonic cooling followed by a high-temperature impact event that introduced silicates into the metal and a low-temperature impact event that partially converted thopyroxene into low-Ca clinopyroxene.

Wasson, John T.↗
NASA NTRS1988

High temperature regenerative H.sub.2 S sorbents

Efficient, regenerable sorbents for removal of H.sub.2 S from high temperature gas streams comprise porous, high surface area particles. A first class of sorbents comprise a thin film of binary oxides that form a eutectic at the temperature of the gas stream coated onto a porous, high surface area refractory support. The binary oxides are a mixture of a Group VB or VIB metal oxide with a Group IB, IIB or VIII metal oxide such as a film of V-Zn-O, V-Cu-O, Cu-Mo-O, Zn-Mo-O or Fe-Mo-O coated on an alumina support. A second class of sorbents consist of particles of unsupported mixed oxides in the form of highly dispersed solid solutions of solid compounds characterized by small crystallite size, high porosity and relatively high surface area. The mixed oxide sorbents contain one Group IB, IIB or VIIB metal oxide such as copper, zinc or manganese and one or more oxides of Groups IIIA, VIB or VII such as aluminum, iron or molybdenum. The presence of iron or aluminum maintains the Group IB, IIB or VIIB metal in its oxidized state. Presence of molybdenum results in eutectic formation at sulfidation temperature and improves the efficiency of the sorbent.

Flytani-Stephanopoulos, Maria↗
NASA NTRS2000

Float processing of high-temperature complex silicate glasses and float baths used for same

A float glass process for production of high melting temperature glasses utilizes a binary metal alloy bath having the combined properties of a low melting point, low reactivity with oxygen, low vapor pressure, and minimal reactivity with the silicate glasses being formed. The metal alloy of the float medium is exothermic with a solvent metal that does not readily form an oxide. The vapor pressure of both components in the alloy is low enough to prevent deleterious vapor deposition, and there is minimal chemical and interdiffusive interaction of either component with silicate glasses under the float processing conditions. Alloys having the desired combination of properties include compositions in which gold, silver or copper is the solvent metal and silicon, germanium or tin is the solute, preferably in eutectic or near-eutectic compositions.

Cooper, Reid Franklin↗
NASA NTRS2009

Fused Bead Analysis of Diogenite Meteorites

Bulk rock chemistry is an essential dataset in meteoritics and planetary science [1]. A common method used to obtain the bulk chemistry of meteorites is ICP-MS. While the accuracy, precision and low detection limits of this process are advantageous [2], the sample size used for analysis (approx.70 mg) can be a problem in a field where small and finite samples are the norm. Fused bead analysis is another bulk rock analytical technique that has been used in meteoritics [3]. This technique involves forming a glass bead from ~10 mg of sample and measuring its chemistry using a defocused beam on a microprobe. Though the ICP-MS has lower detection limits than the microprobe, the fused bead method destroys a much smaller sample of the meteorite. Fused bead analysis was initially designed for samples with near-eutectic compositions and low viscosities. Melts generated of this type homogenize at relatively low temperatures and produce primary melts near the sample s bulk composition [3]. The application of fused bead analysis to samples with noneutectic melt compositions has not been validated. The purpose of this study is to test if fused bead analysis can accurately determine the bulk rock chemistry of non-eutectic melt composition meteorites. To determine this, we conduct two examinations of the fused bead. First, we compare ICP-MS and fused bead results of the same samples using statistical analysis. Secondly, we inspect the beads for the presence of crystals and chemical heterogeneity. The presence of either of these would indicate incomplete melting and quenching of the bead.

Mittlefehldt, D.W.↗
NASA NTRSDate not supplied

Computational Tools to Design Molten Salt Electrolytes for High-Temperature Environments

Current Li-ion batteries are designed for a small operating window of 5 °C to 55 °C. Modifications to the electrolyte for operation in Mars atmosphere extended this range on the lower bound to ~ -40 °C. These operating-temperature ranges are far from those presented in high-temperature environments, such as the Venus surface, where temperatures are around 450 °C. Protecting the state-of-the-art Li-ion batteries require insulations that decreases the volumetric capacity and limiting the operational time-window. These unique challenges require a paradigm shift in materials used for designing high-temperature batteries. Molten salt electrolyte-based batteries offer a plausible route to designing high-temperature batteries. ZEBRA batteries are known to be one of the safest energy storage devices operating at 270-350 °C. Nitrate based eutectics, operating at 150 °C have also been used in Li-O2 batteries. In this study, we will examine molten-salt electrolyte transport and electrochemical properties using first-principles computations and benchmark against experiments. Further, we will present thermodynamics-based models for designing and predicting melting point of molten salt mixtures. Based on these computational tools, new molten salt mixtures designed with desired operating temperatures and electrochemical windows will be presented. Implications of these new eutectics in the context of high-temperature environment exploration will also be discussed.

Balachandran Radhakrishnan↗
DOE OSTI2017

Microanalysis of Irradiated Metallic Hydride Nuclear Fuel (U{sub 0.17}ZrH{sub 1.6})

Metallic hydride nuclear fuels (U{sub 0.17} ZrH{sub 1.6}) have been under consideration for use in Light Water Reactors (LWRs). The fuel matrix consists of isolated particles of uranium metal within a zirconium hydride matrix. Erbium was also added as a neutron poison enabling higher reactor performance. These fuels were encased in a Zircaloy-2 cladding with a Bi/Pb eutectic liquid metal filled-gap to improve thermal conductivity. The inner and outer cladding surfaces were oxidized to nominal 1 μm thickness to eliminate hydrogen attack. The fuels were termed UCB to note the location of fabrication as the University of California-Berkeley. Irradiations were performed in the MITR research reactor. The details are described elsewhere. We originally reported on post-irradiation analysis of the fuel elements of two of the rodlets using Scanning Electron Microscopy (SEM) and x-ray energy dispersive spectroscopy (EDS). In this further study, funded as a rapid turnaround experiment (RTE) through the Nuclear Science User Facilities (NSUF) program, we performed high-resolution Scanning Transmission Electron Microscopy (STEM) of thin lift-out specimens prepared from specific regions in the fuel matrix using an SEM-Focused Ion Beam (FIB) instrument, and again compared these results to the unirradiated material. Earlier investigations using SEM-EDS showed that ∼8% of the Zircaloy cladding had dissolved in the Pb-Bi eutectic during irradiation over 1000 hrs. However, the SEM-EDS failed to show any detectable evidence of damage of the fuel matrix. There was no obvious swelling or migration of elements; hence, we focused on these specific regions in greater detail. Much of the data on hydride fuels come from the Space Nuclear Auxiliary Power (SNAP) program from the 1960's. The principle difference between oxide and hydride fuel is the high thermal conductivity of the latter. This feature greatly decreases the temperature drop over the fuel during operation, thereby reducing the release of fission gases to the fraction due only to recoil. However, very unusual early swelling due to void formation around the uranium metal particles has been reported in hydride fuels over 700 deg. C. In this investigation, the fuel did not reach these extreme temperatures. Phases formed in this system have been previously experimentally investigated using thermal analysis techniques, and wavelength and energy dispersive spectroscopy (EDS/WDS) in scanning electron microscopes (SEM). Major changes were observed in the liquid metal and cladding components but at the scale of the SEM observations, it was not readily apparent that any major changes had occurred to the fuel matrix (i.e. U metal particles in the zirconium hydride matrix with interdispersed erbium metal). Rapid oxidation of the SEM mechanically polished cross-sections, may have obscured our ability to see major changes. By using the SEM-FIB slices, it was possible to remove oxide coatings and the smoother surfaces were found to be less susceptible to oxidation once removed from the vacuum chamber. The high spatial resolution of STEM allowed characterization of individual matrix phases.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2024

Elucidating the corrosion mechanism of commercial Ni-based Superalloys in UCl3 containing-chloride Molten Salt Systems

Molten salt reactors (MSRs) have gained renewed interest, providing several advantages over their predecessors, including the capability to consume spent fuels, enhancing the environmental sustainability of the uranium fuel cycle. For example, molten chloride fast reactors (MCFRs) can reach criticality with molten chloride spent fuel containing high concentrations of impurities, such as actinide products like uranium chloride (UCl3). However, the redox potential of chloride molten salt fuels may change in the presence of these impurities, dictating their corrosivity and in turn the corrosion performance of structural components, such as those constructed from nickel (Ni)-based alloys. The purpose of this investigation is to assess the extent of corrosion of Ni-based alloy, Inconel 617, when exposed to UCl3-LiCl-KCl eutectic salt. Inconel 617 one of only six structural materials that are fully qualified by the American Society for Mechanical Engineers (ASME) Boiler and Pressure Vessel Code for high-temperature nuclear reactor components, making it a technologically mature material to consider for constructing MCFRs. Inconel 617 specimens were submerged in a static LiCl-KCl-UCl3 eutectic salt mixture heated at 700 C for 1000 h under an inert atmosphere. Upon completion, the extent of corrosion was analyzed through a multi-modal characterization approach spanning the engineering to nanoscale, employing computed tomography, focused-ion beam, and transmission electron microscopy techniques. Results from this investigation will enhance our understanding of property-to-performance relationships of candidate structural materials for MSRs with respect to corrosion resistance and interactions between the salt and alloy interface.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Activity coefficient acquisition with thermodynamics–informed active learning for phase diagram construction

This work explores the use of thermodynamics-informed Gaussian processes (GPs) and active learning (AL) to model activity coefficients and construct phase diagrams. Relying on synthetic data generated from an excess Gibbs energy model, GPs were found to accurately describe the activity coefficients of several binary mixtures across large composition and temperature ranges. Moreover, GPs could estimate their own uncertainty and identify composition/temperature regions where activity coefficient data provide the most information to the models. This was leveraged to build AL algorithms targeted at modeling phase equilibria. In many cases, a single active-learning-acquired data point was sufficient to describe the phase diagrams studied. Lastly, the ability of AL to greatly reduce the amount of data needed to obtain accurate models was further verified on experimental case studies, namely individual ion activity coefficients, the solid–liquid and vapor–liquid equilibrium of deep eutectic solvents, and phase equilibria in ternary mixtures.

25 ENERGY STORAGE↗
DOE OSTI2025

Kinetic Investigation by Batch Processing of Film Growth during the Electrodeposition of Titanium from Ethaline

Titanium electrodeposition as a technological advance has been out of reach due to the poor film quality obtained when using previously developed methods. This study shows that the electrodeposition of Ti is possible and feasible from the deep eutectic solvent ethaline. Moreover, this study shows through batch analysis that this deposition has temperature-dependent aspects that alter the film deposition kinetics upon modest heating. This ultraviolet–visible spectroscopic study is highlighting the more facile reduction of Ti 4+ to Ti 3+ and then to Ti 2+ at elevated temperatures. Understanding the underlying kinetics of electrodeposition opens up new venues for the application of this important metal.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Ozone Generator Aluminum Electrode Soldering

The creation of an entirely soldered ozone electrode component is proposed and implemented for the first time by the authors. Electrode construction with a ribbed plate insert within it is the most perfect heat exchange device from the point of view of effective heat exchange and uniform distribution of liquid flow through its section. Stages are considered for electrode preparation for soldering and a standard heating cycle is proposed for soldering and electrode with eutectic silumin. It is shown that as a result of the soldering thermal cycle metal structure becomes coarse-grained and favorable for subsequent electrochemical formation of a nanostructured anodic oxide coating 50–60 μm thick.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2023

Microstructural refinement in ultrasonically modified A356 aluminum castings

Two A356 aluminum alloys (Al-Si-Mg), one with 0.09 wt.% Fe and one with 0.91 wt.% Fe, were cast in a graphite mold with the simultaneous application of local ultrasonic intensification to refine the as-cast microstructure. Ultrasonication during casting transformed the morphology of primary Al grains from dendritic (~140-290 microns in size) to globular (~33-36 microns in size). The alloy with high Fe exhibited globular grains at distances up to 45 mm away from the ultrasound probe, while the alloy with low Fe exhibited globular grains at distances only up to 6 mm away from the ultrasound probe. Near the location of the ultrasound probe (< 2 mm away), a second non-dendritic microstructural morphology was observed with fine aluminum grains (~9-25 microns in size). This unique fine-grained morphology has not been previously reported, contains a greater concentration of Si relative to the globular microstructure, and may be a large, fully eutectic region. Ultrasonication during casting also transformed the morphology of the ß-Al 5 FeSi phase particles (which are deleterious to the strength and ductility of the alloy) in the high Fe alloy from needle-like to rectangular, which could enable the greater use of secondary Al alloys. Thermodynamic simulations conducted to calculate the solidification paths of the two alloys studied predict that the ß-Al 5 FeSi phase begins to form earlier in the alloy with high Fe. Finally, data suggest that the ß-Al 5 FeSi phase (which is more abundant in alloys with high Fe content) may enhance ultrasonically-induced grain refinement.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Hydrogen sorbing magnesium alloys and composites

The authorsr works studying the hydrogen sorption properties of the magnesium-based materials are reviewed. The objects of the studies were highly dispersed powders of Mg—La—Ni and Mg—Mm—Ni alloys (Mm is misch metal) of the ternary eutectic, composites of magnesium alloys with extended carbon nanostructures, and composites of magnesium hydride with lanthanide oxides. The positive effect of lanthanide oxide additives on the process of hydro-gen desorption from magnesium hydride and the role of carbon nanofibers in these processes carried out at room temperatures are discussed.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2018

Electrical and Thermal Conductivity of Solid Solution Sn{sub 1–x}Mn{sub x}Te (0 ≥ x ≥ 0.04)

Electrical and thermal properties of the Sn{sub 1–x}Mn{sub x}Te single crystals (0 ≥ x ≥ 0.04) with contacts of eutectic alloy 57Bi + 43Sn (in mass%) are investigated at temperatures from 77 to 300 K. Experimental results show that this alloy with specified single crystals forms ohmic contact with a sufficiently low contact resistance. The electronic thermal conductivity in some samples reaches about 50% of the total thermal conductivity, and structural defects contribute significantly to the thermal resistance of the crystals.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2017

Use of Friction Stir Processing for Improving Heat-Affected Zone Liquation Cracking Resistance of a Cast Magnesium Alloy AZ91D

In this work, a cast magnesium alloy AZ91D was friction stir processed. Detailed microstructural studies and Gleeble hot ductility tests were conducted on the as-cast and the FSPed samples to comparatively assess their heat-affected zone liquation cracking behavior. The results show that the use of FSP as a pretreatment to fusion welding can strikingly improve the heat-affected zone liquation cracking resistance of alloy AZ91D by reducing the amount and size of the low-melting eutectic β (Mg{sub 17}Al{sub 12}) as well as by refining the matrix grain size.

36 MATERIALS SCIENCE↗