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At least 667 records · Page 37
All sourcesNASA NTRSDOE OSTI
NASA NTRS2019

Remarkable Diversity of Refractory Inclusions in the Miller Range 090019 CO3.1 Chondrite

We have characterized the mineralogy, textures, bulk compositions, modal abundances and some mineral compositions in a suite of approximately 140 refractory inclusions from the MIL090019 carbonaceous chondrite. All of these 140 inclusions are found in a single thin section of this CO3.1 chondrite. These inclusions range from grossite- and hibonite-rich varieties, melilite-, spinel-, fassaite-diopside- and anorthite-rich types, and include a subset of aluminous AOAs (amoeboidal olivine aggregates). Grossite- and hibonite-bearing inclusions were discussed briefly in previous abstracts. X-ray mapping by energy dispersive spectrometry has permitted us to extract the bulk compositions of these inclusions from hyperspectral x-ray datasets. The bulk compositions of these inclusions represent the full range of recognized CAI (Calcium-Aluminum–rich Inclusions) types.

Ross, D. Kent↗
NASA NTRS2020

Isotopic and Microstructural Analyses of Opaque Mineral Assemblages and Their Alteration Products Hosted in a Refractory Inclusion

Calcium-aluminum-rich inclusions (CAIs) hosted in primitive meteorites are the oldest solids formed in the Solar System. Some CAIs contain metal nuggets that are complex assemblages of Fe-Ni alloys, along with rare ultra-refractory metals such as platinum group elements (PGEs), and their alteration products such as magnetite, sulfides, and phosphates. Three possible mechanisms proposed to explain the origin of these metal nuggets include condensation in circumstellar settings, condensation in the solar nebula within the CAI-forming region, or crystallization from immiscible metal-silicate melt. However, secondary alteration processes may have also affected some of these assemblages. Additionally, similar metal assemblages observed in chondrules and chondritic matrix indicate that all of these metal nuggets could share common high-temperature origins. These metal assemblages record early Solar System conditions that are reflected in their distinctive chemical composition, mineralogy and microstructures. Here we report a detailed mineralogical, microstructural and oxygen isotopic study of one such metal assemblage hosted in a CAI to understand the physical and chemical settings in which it formed.

Mane, P.↗
NASA NTRS2022

Ab initio Screening of Refractory Nitrides and Carbides for High Temperature Hydrogen Permeation Barriers

Density functional theory was used to screen eleven refractory materials – two pure metals, six nitrides, and three carbides–as high-temperature hydrogen permeation barriers to prevent hydrogen embrittlement. Activation energies were calculated for atomic hydrogen (H) diffusion into the first subsurface layer from the lowest energy surface of the high-temperature phase of each candidate material. The candidate barrier materials with the highest activation energies are h-BN, c-BN, HfN, and ZrN with predicted barriers of 3.25 eV, 3.23 eV, 3.14 eV, and 2.76 eV, respectively. Strain energies, Bader charges, and density of states were calculated for the diffusing H at the relaxed initial state and the transition state to provide insight into contributing factors to high energy barriers. The diffusing H atom in materials with the highest predicted barriers are protic. In addition, interstitial H atoms induce mid-gap states in the density of states of both BN polymorphs. The nitrogen retention of each nitride material at high temperatures was predicted using nitrogen vacancy formation energies with respect to gaseous nitrogen. Experimental evaluation of nitrogen retention in h-BN, ZrN, and TiN confirmed their resistance to nitrogen loss at 1773 K. However, of these nitrides, TiN is predicted to be the least stable. This work identifies multiple promising materials that are predicted to be effective hydrogen barriers at high temperatures and that are stable at temperatures above 2700 K, with BN predicted to perform best.

Density Functional Theory (DFT)↗
NASA NTRSDate not supplied

Oxygen Isotopic Composition of Refractory Inclusions from the Miller Range (MIL) 090019 Carbonaceous Chondrite

Introduction: Primitive meteorites contain Calcium-Aluminum-rich Inclusions (CAIs)that preserve the records of the earliest times in the Solar System. CAIs record O isotopic variations with time and/or location from solar (16O-rich) to planetary (16O-poor) compositions [e.g., 1, 2].However, CAIs were also affected by parent body processing to varying degrees. The goal of this work was to identify the processes that resulted in the fine-scale spatial variations in oxygen isotopic compositions within the most ancient Solar System solids. We report oxygen isotopic composition of CAIs from MIL 090019 CO3.1 carbonaceous chondrite. MIL 090019 contains a high abundance of CAIs showing mineralogical as well as textural variations [3]. Methods: We analyzed 10 CAIs with different mineralogical assemblages, classified as corundum-bearing, grossite-bearing, hibonite-bearing, melilite-bearing, anorthite-bearing inclusions and amoeboid olivine aggregates(AOA’s). The mineralogical and petrological characterization of CAIs was performed using the JOEL Hyperprobe 8530 electron microprobe at NASA JSC. Oxygen isotopic imaging of the CAIs was done using the Cameca NanoSIMS 50L ion microprobe at NASA JSC. We followed the analytical protocol described in [4]. O-isotopic maps of the CAI were acquired by rastering a ~3 pA primary Cs+beam at 16 keVover an area of 20 ×20μm2over a period of ~7 hours. Negative secondary ions of 16O−, 17O−, 18O−, 28Si−, 24Mg16O−, 27Al16O−, and 40Ca16O−were simultaneously acquired using electron multiplier detectors at a mass resolving power sufficient to resolve the 16OH−interference from the 17O−peak, where the contribution of 16OH−was <0.1%.An electron flood gun was used to mitigate sample charging during the analyses. We used San Carlos olivine and Madagascar hibonite as isotopic standards to correct for the instrumental mass fractionation. The O-isotopic ratios were corrected for the quasi simultaneous arrival (QSA) effect and the detector dead time. All reported errors are 1 sigma. Results: The MIL 090019 carbonaceous chondrite hosts refractory inclusions varying in their mineralogies and textures[2, 3]. We found the oxygen isotopic compositions of mineral phases in MIL 090019 CAIs show large variations with Δ17O values varying from -27 to 0‰. A corundum-bearing inclusion records isotopic variations with corundum, melilite, perovskite, and anorthite showing Δ17Ovalues of -20 ±2.5, -10.2 ± 6.5, -10.7 ± 1.3,and -1.2 ± 3.2‰ respectively. A grossite-hibonite-bearing inclusion also records O-isotopic heterogeneity, where grossite, hibonite, Mg-rich spinel, and melilite show -3.7 ± 2.7, -22.9 ± 2.5, -21.4 ± 2.6, and -17.3 ± 2.8‰ respectively, whereas perovskite grains record a heterogenous isotopic composition ranging from -22.6 to -13.9‰. A hibonite-bearing inclusion shows average Δ17Ο values of -17.6 ± 5.3 ‰ and -15.1 ± 4.8 ‰ for hibonite and spinel respectively. The two perovskite grains also show relatively 16O-poor composition (Δ17Ο = -11.8 ± 6.4 ‰ and -8.6 ± 5.2 ‰). Anorthite has ~0.1 wt% Na2O and ~0.52 wt% FeO and a Δ17Ο value of -7.2 ± 5.0 ‰, whereas diopside records a Δ17Ο value of -3.5 ± 5.0 ‰. A hibonite-spinel-rich inclusion contains spinel and hibonite that are16O-rich (Δ17Οvalues -21.3 ± 2.8‰ and -19.4 ± 3.0‰, respectively). Melilite shows heterogenous oxygen isotopic composition, with an inner 16O-rich region and an outer 16O-poor region separated by a sharp boundary, with a bulk Δ17Ο= -16.2 ± 2.1‰, whereas two perovskite grains are relatively 16O-poor (Δ17Ο= -13.2 ± 3.7‰ and -7.1 ± 3.4‰).A spinel-rich inclusion contains perovskite grains with Δ17Οranging from -27.0 to -22.8 ‰and spinel with average Δ17Οvalue of -21.4 ± 2.8 ‰. In a melilite and spinel-rich CAI, perovskite, spinel, diopside, melilite, and Al-Ti-rich pyroxene record Δ17Ο values of-26.9 ± 4.6‰, -22.4 ± 4.3‰,-23.4 ± 4.9, -19.3 ± 3.4, and -19.0 ± 4.3 ‰ respectively. Olivine and spinel components of 2 AOA’s record a 16O-rich composition with Δ17O~-23‰. Discussion: The coexistence of 16O-rich and 16O-poor minerals within CAIs has been attributed to differing degrees of O isotopic exchange, reflecting a wide range of O diffusion rates[5]. However, the O isotopic heterogeneity observed in these CAIs cannot be explained by oxygen diffusion in nebular or parent body settings alone. The isotopic imaging of CAIs from the MIL 090019 meteorite shows variations in the O isotopic composition recorded in their mineral components, suggesting that these CAIs record the oxygen isotopic heterogeneity in the nebular gas from which they condensed. The coexistence of 16O-rich and 16O-poor mineral components in the CAI-forming region suggests that the gas in this region was not well-mixed and consisted of distinct 16O-rich and 16O-poor gaseous reservoirs.

P Mane↗
NASA NTRSDate not supplied

Refractory Carbides for Hydrogen Erosion Resistance in Carbon Tubes for Nuclear Thermal Propulsion

As crewed travel becomes more common to the Moon and beyond, space nuclear propulsion-based craft offer reduced travel times and double the specific impulse compared to conventional chemical rockets. The nuclear core and its integral hydrogen propellant channels will require advanced refractory carbide coatings over a carbon/carbon substrate for hydrogen resistance. Using ab initio and other computational techniques, we studied select (Zr/Ta/Nb)C mixed carbide systems for erosion resistance and hydrogen diffusion using realistic levels of carbon vacancies and experimentally obtainable stoichiometries. Various contributions to the formation and hydrogen erosion free energies were calculated, including configurational, electronic, and vibrational terms. Our calculations indicate that ZrC is less likely to lose carbon than NbC or TaC, providing an explanation for heritage NERVA data on ZrC and NbC mass loss performance. Additionally, binary mixtures show compositions that are more stable than their end-member counterparts. Hydrogen diffusion in stoichiometric ZrC was found to be slightly higher than previously theorized, with the caveat that hydrogen saturation of carbon vacancies will hinder further hydrogen diffusion through the bulk, while hydrogen diffusion in ZrNbC is slightly enhanced over ZrC. And finally, we show that as carbon is depleted, the deformation mechanism of ZrC changes from brittle to ductile. Though many questions still remain as to the bulk performance of these materials, these trends and results are important in terms of materials selection efforts for hydrogen-resistant coatings on carbon/carbon substrates.

William C Tucker↗
NASA NTRSDate not supplied

Mineralogical and Oxygen Isotopic Study of Grossite-Bearing Refractory Inclusions From Reduced CV Chondrites

Grossite (CaAl4O7) is predicted to condense as the third major phase, after corundum and hibonite, from a cooling gas of solar composition. Thus, this refractory phase likely preserves a crucial record of high-temperature conditions in the early solar nebula. However, grossite is relatively rare in CAIs from most carbonaceous chondrite groups, except for CH chondrites. Only six grossite-bearing CAIs were reported and studied from CV chondrites, and most of them were coarse-grained Type A inclusions. Our previous study reported the occurrence of six grossite-bearing, fine-grained Ca-Al-rich inclusions (FGIs) from reduced CV chondrites Efremovka, Thiel Mountains (TIL) 07003, and TIL 07007. Here we present oxygen isotopic data of grossite-bearing FGIs from reduced CV chondrites to determine if any oxygen isotopic heterogeneity occurs within and among these inclusions. This isotopic study was coordinated with a FIB/TEM study to examine the formation and alteration history of grossite-bearing FGIs in the early solar nebula and on the asteroidal parent body.

J. Han↗
NASA NTRSDate not supplied

Al-Mg Isotopic Constraints on the Condensation Age of Fine-Grained Refractory Inclusions in Reduced Cv3 Chondrites

Fine-grained Ca-Al-rich inclusions (FGIs) in carbonaceous chondrites are interpreted as aggregates of direct condensates from the solar nebula that escaped extensive melting. Thus far, a few high-precision SIMS Al-Mg chronology studies of FGIs from CV3 chondrites have been reported. Argued that (26Al/27Al)0 of all FGIs are close to the bulk refractory inclusion value of ~5.2×10−5 which may define a time zero for the FGI condensation. A similar (26Al/27Al)0 value was also inferred from an amoeboid olivine aggregate (AOA), which also represents a direct condensate from the solar nebula. In contrast, reported significant variations in (26Al/27Al)0 of FGIs, ranging from ~5.2×10−5 to ~3.4×10−5, and concluded that their formation continued over at least ~0.4 Ma after the canonical value. These contrasting results suggest that the chronological significance for the formation age spread of FGIs in CV3 chondrites is still poorly constrained.

J. Han↗
NASA NTRSDate not supplied

Refractory Carbides for Hydrogen Erosion Resistance in Carbon Tubes for Nuclear Thermal Propulsion

As crewed travel becomes more common to the Moon and beyond, space nuclear propulsion-based craft offer reduced travel times and double the specific impulse compared to conventional chemical rockets. The nuclear core and its integral hydrogen propellant channels will require advanced refractory carbide coatings over a carbon/carbon substrate for hydrogen resistance. Using \textit{ab initio} and other computational techniques, we studied select (Zr/Ta/Nb)C mixed carbide systems for erosion resistance and hydrogen diffusion using realistic levels of carbon vacancies and experimentally obtainable stoichiometries. Various contributions to the formation and hydrogen erosion free energies were calculated, including configurational, electronic, and vibrational terms. Our calculations indicate that ZrC is less likely to lose carbon than NbC or TaC, providing an explanation for heritage NERVA data on ZrC and NbC mass loss performance. Additionally, binary mixtures show compositions that are more stable than their end-member counterparts. Hydrogen diffusion in stoichiometric ZrC was found to be slightly higher than previously theorized, with the caveat that hydrogen saturation of carbon vacancies will hinder further hydrogen diffusion through the bulk, while hydrogen diffusion in ZrNbC is slightly enhanced over ZrC. And finally, we show that as carbon is depleted, the deformation mechanism of ZrC changes from brittle to ductile. Though many questions still remain as to the bulk performance of these materials, these trends and results are important in terms of materials selection efforts for hydrogen-resistant coatings on carbon/carbon substrates.

William C. Tucker↗
NASA NTRSDate not supplied

Refractory Carbides for Hydrogen Erosion Resistance in Carbon Tubes for Nuclear Thermal Propulsion

As crewed travel becomes more common to the Moon and beyond, space nuclear propulsion-based craft offer reduced travel times and double the specific impulse compared to conventional chemical rockets. The nuclear core and its integral hydrogen propellant channels will require advanced refractory carbide coatings over a carbon/carbon substrate for hydrogen resistance. Using ab initio and other computational techniques, we studied select (Zr/Ta/Nb)C mixed carbide systems for erosion resistance and hydrogen diffusion using realistic levels of carbon vacancies and experimentally obtainable stoichiometries. Various contributions to the formation and hydrogen erosion free energies were calculated, including configurational, electronic, and vibrational terms. Our calculations indicate that ZrC is less likely to lose carbon than NbC or TaC, providing an explanation for heritage NERVA data on ZrC and NbC mass loss performance. Additionally, binary mixtures show compositions that are more stable than their end-member counterparts. Hydrogen diffusion in stoichiometric ZrC was found to be slightly higher than previously theorized, with the caveat that hydrogen saturation of carbon vacancies will hinder further hydrogen diffusion through the bulk, while hydrogen diffusion in ZrNbC is slightly enhanced over ZrC. And finally, we show that as carbon is depleted, the deformation mechanism of ZrC changes from brittle to ductile. Though many questions still remain as to the bulk performance of these materials, these trends and results are important in terms of materials selection efforts for hydrogen-resistant coatings on carbon/carbon substrates.

William C Tucker↗
NASA NTRS2024

Thermal Modeling and Testing of High-Temperature Refractory Ceramic Insulation Felts

Heat transfer in high-temperature, high-porosity, flexible refractory ceramic fibrous insulation felts is investigated. Heat transfer in these insulation materials consists of combined gas conduction, solid conduction, and radiation modes, with the precise theoretical modeling of the latter two modes being formidable. A semi-empirical model that requires inverse methods and steady-state thermal test data to infer some of the required model parameters is further developed in this study, and applied to five insulation materials for temperatures between 300 K and 1900 K. The steady-state thermal test setup at NASA Langley Research Center with recent modifications to increase its testing capability to 1900 K is discussed. Design considerations to ensure one-dimensional heat transfer in the test setup are described. Test data and corresponding thermal models for alumina and zirconia-based fibrous insulation felts are presented. Furthermore, test data and thermal models on two fibrous insulation samples containing additives to further suppress either radiation or gas conduction modes of heat transfer are presented. Previously published alumina-based insulation data are also re-processed using the updated modeling methodology. The significance of various heat transfer modes in typical insulation samples is discussed and used to provide general guidance on optimum insulation layups.

Kamran Daryabeigi↗
NASA NTRS2024

A Coordinated Mineralogical and Oxygen Isotopic Study of Refractory Ca-Al-Rich Inclusions

Refractory Ca-Al-rich inclusions (CAIs) in primitive chondritic meteorites represent the oldest solids that formed in our Solar System. Coordinated analyses using multiple ion and electron-beam techniques are vital to fully understand complex nebular and asteroidal processes that CAIs may have experienced in the context of the formation and early evolution of our Solar System. We report the results of a coordinated mineralogical and oxygen isotopic study of unique grossite bearing CAIs from reduced CV (Vigarano type) carbonaceous chondrites using transmission electron microscopy and secondary ion mass spectrometry. Grossite (CaAl 4 O 7 ) occurs in cores of nodules in fine grained CAIs that likely represent aggregates of nebular condensates. In many occurrences, grossite has been partially replaced by hercynite [(Fe,Mg,Zn)Al 2 O 4 ], which displays complex microstructures and compositions, and magnetite nanoparticles. This grossite alteration likely occurred via crystallographically controlled metasomatic reactions with Zn, Fe-rich aqueous fluids on the parent asteroid. The constituent phases of grossite bearing CAIs show heterogeneous oxygen isotopic compositions . That is, grossite and perovskite are 16 O poor and melilite is variably 16 O-depleted in contrast to solar like, 16 O-rich hibonite and spinel. The observed oxygen isotopic distribution is interpreted as a result of mineralogically controlled oxygen isotopic exchange with an 16 O-poor fluid on the parent asteroid. Collectively, we conclude that the presence of limited fluids played an important role in preferential alteration of grossite to hercynite and magnetite and various degrees of 16 O depletion in grossite, perovskite, and melilite during thermal metamorphism on the CV chondrite parent asteroid.

Jangmi Han↗
DOE OSTI2019

Electroless process for depositing refractory metals

The invention provides an inexpensive, scalable process for coating materials with a film of a refractory metal. As an example, the immersion process can comprise the deposition of a sacrificial zinc coating which is galvanically displaced by the ether-mediated reduction of oxophilic WCl6 to form a complex WOxCly film, and subsequently annealed to crystalline, metallic tungsten. The efficacy of this process was demonstrated on a carbon foam electrode, showing a 50% decrease in electrode resistance and significant gains in electrochemical performance. This process enables voltage efficiency gains for electrodes in batteries, redox flow batteries, and industrial processes where high conductivity and chemical stability are paramount.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Stability of refractory materials in high temperature steam

The present invention relates, in part, to a discovery of a method for using atomic layer deposition (ALD) to improve the stability of refractory materials in high temperature steam, and compositions produced by the method.

Weimer, Alan W.↗
DOE OSTI2025

REFRACTORY COMPACT HEAT EXCHANGERS WITH EMBEDDED SENSORS ENABLED BY HYBRID ADVANCED SINTERING AND ADDITIVE APPROACH

Structural health monitoring (SHM) of compact heat exchangers (CHXs) operating in extreme environments is essential for ensuring system reliability, safety, and longevity. This study presents the development of high-temperature sensors fabricated via aerosol jet printing (AJP) using platinum ink, selected for its exceptional thermal stability, oxidation resistance, and electrical conductivity. AJP enables precise deposition of fine-feature sensor patterns onto complex geometries, making it well-suited for integration within CHX architectures. To enhance sensor durability, an alumina-based ceramic protective layer was printed over the platinum sensing elements. The sensors demonstrated stable, repeatable performance up to 900?°C during extended thermal cycling. A custom test setup was developed to evaluate sensor accuracy and robustness under steady-state and transient conditions. Substrate screening identified HG-1 ceramic-coated stainless steel as the most effective platform, offering strong adhesion and low resistance. Furthermore, electric field-assisted sintering (EFAS) was employed to embed the sensors into stainless steel 316L matrices without degrading their functionality. Post-embedding electrical tests confirmed sensor integrity, and initial characterization suggests strong potential for in-situ monitoring. This work provides a scalable strategy for integrating high-performance temperature sensors directly into refractory components, advancing embedded SHM technologies for harsh operating environments.

36 - MATERIALS SCIENCE↗
DOE OSTI2026

Mechanical Behavior of Neutron Irradiated Refractory Multi-Principal Element Alloys Processed via Spark Plasma Sintering

The search for advanced materials capable of withstanding the extreme conditions of Generation IV reactors is a critical area in materials science research. These reactors operate under severe environments, including high temperatures, corrosion, stress, and irradiation damage. Consequently, there is a need for innovative alloy systems to ensure the reliability and longevity of proposed Generation IV reactor components. Refractory multi-principal-element alloys (RMPEA) have emerged as a promising candidate due to their exceptional properties. These alloys, characterized by their composition of multiple principal elements in near-equiatomic ratios, exhibit superior resistance to irradiation damage, reduced void swelling, enhanced microstructural stability, and minimal irradiation-induced hardening. While initial studies on RMPEAs have shown promising results, most research has been limited to thin films, nanocrystalline microstructures, and ion irradiation, which do not accurately represent the behavior of bulk materials. To address this gap, our research focused on the neutron irradiation of bulk RMPEAs. We aim to conduct comprehensive post-irradiation examinations (PIE) of RMPEAs irradiated at the Advanced Test Reactor at Idaho National Laboratory. The RMPEAs were synthesized using spark plasma sintering (SPS) with mechanically alloyed metallurgical powder. The RMPEA specimens are a MoNbTi alloy system with additions of -Zr, and -ZrV. Furthermore, PIE consisted of mechanical testing and advanced materials characterization. The mechanical testing consisted of sub-sized tensile testing, micro- and nano- indentation. Microstructural characterization included scanning electron microscopy and transmission electron microscopy. Mechanical testing coupled with advanced microscopy techniques provides insight into phase morphology and its effects on the mechanical properties of the RMPEA specimens. The results indicate that both pristine and irradiated RMPEA specimens exhibited brittle behavior during tensile testing, which can be attributed to their heterogeneous microstructure. The SPS manufacturing process did not include any post treatment, which resulted in a heterogeneous microstructure. Energy-dispersive X-ray spectroscopy revealed the presence of intermetallic such as laves phases within the microstructure. Specifically, Ti-rich precipitates were observed in the MoNbTi specimen, while Mo-rich precipitates were found in the MoNbTiZrV specimen. Nano-hardness testing of pristine samples showed that the laves phases exhibited higher hardness values compared to the matrix phase, suggesting that precipitate hardening is likely the dominant hardening mechanism in these specimens. The results from this work will be used to build a finite element model to predict mechanical behavior of future MPEA compositions. Thus, enabling for a streamlined approach to developing novel MPEAs for the nuclear industry.

36 - MATERIALS SCIENCE↗