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NASA NTRS2015

Early Size Distributions of Chondrule Subgroups Overprinted by the Final Accumulation Process of Particle Components in Allende

Populations of compositionally distinct particles are fundamental components of undifferentiated chondritic meteorites. Many theories explain the formation of chondrites, one class of which includes mechanisms for sorting the component particles in the solar nebula prior to their accretion. Mechanisms include sorting by mass, turbulent concentration, X-winds, and photophoresis, which will produce characteristic distributions of observable properties such as particle size. Distinguishing processes that occur in specific astrophysical environments requires characterization of particle types, which include refractory Ca-Al-rich Inclusions (CAIs) and less-refractory chondrules. Previous investigations of modal abundances of CAIs and chondrules exist, but differences within and between these two groups, both of which are made up of diverse subgroups with different thermal histories and chemical compositions, remain mostly unstudied. The presence of rims, a significant event occurring after the formation of at least some chondrules, have also yet to be considered with respect to sorting. Here we present the sizes of CAIs and chondrules in Allende with attention to the smallest sizes, subgroups, and particle rims.

McCain, K. A.↗
NASA NTRS2015

Assemblage of Presolar Materials and Early Solar System Condensates in Chondritic Porous Interplanetary Dust Particles

Anhydrous chondritic porous inter-planetary dust particles (CP IDPs) contain an assortment of highly primitive solar system components, molecular cloud matter, and presolar grains. These IDPs have largely escaped parent body processing that has affected meteorites, advocating cometary origins. Though the stardust abundance in CP IDPs is generally greater than in primitive meteorites, it can vary widely among individual CP IDPs. The average abundance of silicate stardust among isotopically primitive IDPs is approx. 375 ppm while some have extreme abundances up to approx. 1.5%. H and N isotopic anomalies are common in CP IDPs and the carrier of these anomalies has been traced to organic matter that has experienced chemical reactions in cold molecular clouds or the outer protosolar disk. Significant variations in these anomalies may reflect different degrees of nebular processing. Refractory inclusions are commonly observed in carbonaceous chondrites. These inclusions are among the first solar system condensates and display 16O-rich isotopic compositions. Refractory grains have also been observed in the comet 81P/Wild-2 samples re-turned from the Stardust Mission and in CP IDPs, but they occur with much less frequency. Here we conduct coordinated mineralogical and isotopic analyses of CP IDPs that were characterized for their bulk chemistry by to study the distribution of primitive components and the degree of nebular alteration incurred.

Nguyen, A. N.↗
NASA NTRS2016

Abundant Solar Nebula Solids in Comets

Comets have been proposed to consist of unprocessed interstellar materials together with a variable amount of thermally annealed interstellar grains. Recent studies of cometary solids in the laboratory have shown that comets instead consist of a wide range of materials from across the protoplanetary disk, in addition to a minor complement of interstellar materials. These advances were made possible by the return of direct samples of comet 81P/Wild 2 coma dust by the NASA Stardust mission and recent advances in microscale analytical techniques. Isotopic studies of 'cometary' chondritic porous interplanetary dust particles (CP-IDPs) and comet 81P/Wild 2 Stardust samples show that preserved interstellar materials are more abundant in comets than in any class of meteorite. Identified interstellar materials include sub-micron-sized presolar silicates, oxides, and SiC dust grains and some fraction of the organic material that binds the samples together. Presolar grain abundances reach 1 weight percentage in the most stardust-rich CP-IDPs, 50 times greater than in meteorites. Yet, order of magnitude variations in presolar grain abundances among CP-IDPs suggest cometary solids experienced significant variations in the degree of processing in the solar nebula. Comets contain a surprisingly high abundance of nebular solids formed or altered at high temperatures. Comet 81P/Wild 2 samples include 10-40 micron-sized, refractory Ca- Al-rich inclusion (CAI)-, chondrule-, and ameboid olivine aggregate (AOA)-like materials. The O isotopic compositions of these refractory materials are remarkably similar to their meteoritic counterparts, ranging from 5 percent enrichments in (sup 16) O to near-terrestrial values. Comet 81P/Wild 2 and CP-IDPs also contain abundant Mg-Fe crystalline and amorphous silicates whose O isotopic compositions are also consistent with Solar System origins. Unlike meteorites, that are dominated by locally-produced materials, comets appear to be composed of materials that were formed across a wide swath of the early protoplanetary disk.

Messenger, S.↗
NASA NTRS2017

A New Type of Foreign Clast in A Polymict Ureilite: A CAI or AL-Rich Chondrule

Introduction: Polymict ureilites are breccias interpreted to represent regolith formed on a ureilitic asteroid [1-3]. They consist of approximately 90-95% clasts of various ureilite types (olivine-pyroxene rocks with Fo 75-95), a few % indigenous feldspathic clasts, and a few % foreign clasts [4-20]. The foreign clasts are diverse, including fragments of H, L, LL and R chondrites, angrites, other achondrites, and dark clasts similar to CC [6,7,9-19]. We report a new type of foreign clast in polymict ureilite DaG 999. Methods: Clast 8 in Dar al Gani (DaG) 999/1 (Museum fur Naturkunde) was discovered during a survey of feldspathic clasts in polymict ureilites [19,20]. It was studied by BEI, EMPA, and X-ray mapping on the JEOL 8530F electron microprobe at ARES, JSC. Petrography and Mineral Compositions: Clast 8 is sub-rounded to irregular in shape, approximately 85 micrometers in diameter, and consists of approximately 68% pyroxene and 32% mesostasis (by area). Part of the pyroxene (top half of clast in Fig. 1a and 2) shows a coarse dendritic morphology; the rest appears massive. Mesostasis may be glassy and contains fine needles/grains of pyroxene. The pyroxene has very high CaO (23.5 wt.%) and Al2O3 (19.7 wt.%), with the formula: (Ca(0.91)Mg(0.63)Fe(0.01)Al(sup VI) (0.38)Cr(0.01)Ti(0.05)1.99 Si2O6. The bulk mesostasis also has very high Al2O3 (approximately 26 wt.%). A bulk composition for the clast was obtained by combining modal abundances with phase compositions (Table 1, Fig. 3). Discussion: The pyroxene in clast 8 has a Ca-Al-(Ti)- rich (fassaitic) composition that is clearly distinct from compositions of pyroxenes in main group ureilites [22] or indigenous feldspathic clasts in polymict ureilites [4-8]. It also has significantly higher Al than fassaite in angrites (up to approximately 12 wt.% [23]), which occur as xenoliths in polymict ureilites. Ca-Al-Ti rich pyroxenes are most commonly found in CAIs, Al-rich chondrules and other types of refractory inclusions in chondrites [21,24-31]. However, the clast 8 pyroxene matches only the most Al-Ca-rich of these, e.g., pyroxenes in type B CAIs in CV3 chondrites [25,30,31], a pyroxene-hibonite spherule and a pyroxene-anorthitespinel fragment from unique CC Acfer 094 [29], and one Al-rich chondrule from Chainpur (LL3.4) [21]. The mineralogy of clast 8 is not consistent with the mineral assemblages of any of these objects (since it lacks hibonite, spinel and/or anorthite), which suggests that it is unrepresentatively sectioned or is a fragment of a more mineralogically diverse object. Its bulk composition (Table 1; Fig. 3) is similar to bulk compositions of some Al-rich chondrules, as well as those of Type C CAIs (which plot in the sp+An+L field in Fig. 3), although it is enriched in silica relative to type C CAIs [e.g., 31]. This suggests a more likely affinity to Al-rich chondrules, although most Al-rich chondrules have less Al-Ca-rich pyroxene [21,26,27]. These bulk compositional comparisons may not be definitive, however, if the clast is unrepresentatively sampled. One of eleven Al-rich chondrules from UOCs described by [21] has textural and compositional characteristics that make it a possible progenitor type for clast 8. This chondrule (Chainpur 1251-14-2) is anorthiteporphyritic, with an interstitial dendritic intergrowth of pyroxene (similar in composition to that in clast 8) and plagioclase [21]. Clast 8 is conceivably a fragment from the interstitial area of such an object. The occurrence of glassy mesostasis (in clast 8) rather than plagioclase may not be a significant difference; it could result from a difference only in cooling rate. Al-rich chondrules with glassy mesostasis are rare, and known occurrences are Ca-poor [26], unlike clast 8. Polymict ureilites are known to contain xenoliths of various chondrites (including OC, R and CC) as well as individual ferromagnesian and silica-pyroxene chondrules probably derived from OC or RC [6,9,15,16,18]. This is the first report of an individual chondritic refractory inclusion as a xenolith in a polymict ureilite. An RC-like sample from anomalous polymict ureilite Almahata Sitta contains CAIs, but they are spinel-rich and not similar to clast 8 [13,14]. Further studies of this clast (which, unfortunately, may not be possible), or the discovery of additional (more representative?) materials of this type would be needed to determine the exact nature of this xenolith and the type of chondrite from which it is derived.

Goodrich, C. A.↗
NASA NTRS2015

Great New Insights from Failed Experiments, Unanticipated Results and Embracing Controversial Observations

Experimental data and observations, whether telescopic or analytical, are never wrong, though data derived from such sources can be misinterpreted or applied inappropriately to derive conclusions that are incorrect. Given that nature always behaves according to the laws of physics and chemistry, rather than according to currently popular models and theories, experimental results should always be considered correct even when the results are far from those that one might initially expect. We discuss a number of cases where the results of experiments, even one carried out as a simple calibration measure, produced wildly different results that generally required many years of effort or contemplation to understand. On the positive side, exploration of the circumstances that produced the errant results often led to new and interesting insights concerning processes that might occur in natural environments and that were well worth the effort involved. Specifically, we show how an experiment that "failed" due to a broken conductor led to experiments that made the first refractory oxide solids containing mass independently fractionated oxygen isotopes and to 1998 predictions of the oxygen isotopic composition of the sun that were confirmed by the analysis of Genesis samples in 2011. We describe a calibration experiment that unexpectedly produced single magnetic domain iron particles. We discuss how tracking down a persistent source of "contamination" in experiments intended to produce amorphous iron and magnesium silicate smokes led to a series of studies on the synthesis of carbonaceous grain coatings that turn out to be very efficient Fischer-Tropsch catalysts and have great potential for trapping the planetary noble gases found in meteorites. We describe how models predicting the instability of silicate grains in circumstellar environments spurred new measurements of the vapor pressure of SiO partially based on previous experiments showing unexpected but systematic non-equilibrium behavior instead of the anticipated equilibrium products resembling meteoritic minerals. We trace the process that led from observations of the presence of crystalline minerals detected in the comae of some comets to the 1999 prediction of large-scale circulation of materials from the hot, innermost regions of the solar nebula out to the cold dark nebular environments where comets form. This large-scale circulation was ultimately confirmed by analyses of highly refractory Stardust samples collected from the Kuiper Belt Comet Wild 2. Finally we discuss a modern and still unresolved conflict between the assumptions built into three well known processes: the CO Self Shielding Model for mass independent isotopic fractionation of oxygen in solar system solids, rapid and thorough mixing within the solar nebula, and the efficient conversion of CO into organic coatings and volatiles on the surfaces of nebular grains via Fischer-Tropsch-type processes.

controversial↗
NASA NTRS2017

Metastable Phase Relations in the System Ca(sub O)-Al2(sub O)3-MgO-TiO(sub 2): Applications to Ca- And Al-Rich Inclusions

Introduction: High temperature phases such as corundum, hibonite, grossite, and perovskite are among the earliest phases that condensed in the early solar nebula. Recent work has shown that defect-structured phases occur in some ultrarefractory inclusions as metastable, possibly more kinetically-favored alternatives to the thermodynamically predicted stable phase assemblages [1-4]. For example, Han et al. have shown that non-stoichiometry in hibonite is accommodated by extra "spinel" blocks in the structure instead of the equilibrium assemblages hibonite+corundum or hibonite+spinel. To explore these relations, we have conducted a series of experiments in the system CaO-Al2O3- MgO-TiO2. Here we discuss the compositions and mineralogy of the experimental samples and how they relate to phases in refractory inclusions with a focus on perovskite and spinel. Methods: For the series of annealing studies, a CaO-Al2O3 eutectic melt is allowed to react with a pure alumina crucible at 1,530degC for either 4 hours or 5 days, followed by quenching in air. Later experiments were similar except that additions of 5 wt% MgO, and CaTiO(sub 3) were used to explore the effect of minor elements on the phase assemblages. The experimental conditions resulted in reaction zones approximately 100-300 m wide consisting of a hibonite layer immediately adjacent to the corundum, followed by a grossite layer, and finally krotite with residual quenched melt. For the experiments with Mg, spinel is distributed in all layers but is mainly concentrated in the krotite layer. In the Ti-bearing experiments, perovskite precipitated in association with the krotite and residual melt. In addition to the experiments, we also analyzed perovskite grains in the FUN inclusion SHAL [5] and a large compact type A CAI from Allende. The experiments and refractory inclusions were analyzed using a JEOL 7600F SEM and quantitative analyses were obtained using the JEOL 8530F field-emission electron microprobe.

Keller, L. P.↗
NASA NTRS2013

Compositions of the Surfaces of Pluto and its Satellites

The information we have on the chemical compositions of the surfaces of Pluto and Charon has been obtained from Earth-based near-infrared spectroscopy. These bodies are seen in diffusely scattered sunlight upon which absorption bands diagnostic of specific ices are superimposed. Identified so far on Pluto are molecular nitrogen (N2), methane (CH4), carbon monoxide (CO), and ethane (C2H6), all in the frozen state. Charon has the clear spectral signature of H2O ice in the crystalline phase, plus an absorption band near 2.2 microns identified as a hydrated form of NH3. No diagnostic spectra of Pluto's other satellites are currently available. A fraction of Pluto's CH4 is dissolved in solid N2, which is in the hexagonal beta-phase. When a small concentration of CH4 exists in a N2 crystalline matrix, its absorption bands are shifted in wavelength by a small but detectable amount. Indeed the shifting of the CH4 bands is diagnostic of a host matrix. In the case of Pluto, the N2 band (2.148 microns) itself is detected, but for other trans-Neptunian objects where the N2 band cannot be seen, the shifted CH4 bands demonstrate the presence of N2 or (less likely) some other spectrally neutral and transparent matrix material (e.g., Ar). The absence of detectable CO2 and H2O ices on Pluto, while they are clearly present on the otherwise very similar Triton, is noteworthy. The ices of Pluto distributed non-uniformly across its surface, and the distribution shows long-term (decadal) changes. Both seasonal and secular changes may be occurring through transport across the surface as a result of changing temperature, and by seasonal changes in the vapor pressure equilibrium of the ice with the tenuous and variable atmosphere. Models of the photochemistry of the surface ices and the atmosphere of Pluto predict the presence of several materials not yet detected; the most abundant photoproducts are expected to be C2H2, C4H2, HCN, C2H6; HCN has been detected on Triton. Both Pluto and Charon have surface components in addition to the detected ices. These materials of presently unknown composition serve to reduce the albedos of both bodies below that expected for pure ices, and in the case of Pluto impart a yellow-brown coloration; the color of Charon is more nearly neutral. It is generally thought that the non-ice components are more refractory than the ices and that they may be complex carbonaceous materials derived from the ultraviolet and charged particle processing of the surface ices. Minerals are also plausible candidates for the non-ice fraction. The refractory colored components may constitute bedrock upon which variable amounts of the ices are alternately deposited and evaporated as the seasons change. Water ice is expected to be a component of the bedrock, although it has not yet been reliably identified.

Pluto↗
NASA NTRS2019

The Evolution of Dust Opacity in Core Collapse Supernovae and the Rapid Formation of Dust in Their Ejecta

Infrared (IR) observations of core collapse supernovae (CCSNe) have been used to infer the mass of dust that has formed in their ejecta. A plot of inferred dust masses versus supernova (SN) ages shows a trend of increasing dust mass with time, spanning a few decades of observations. This trend has been interpreted as evidence for the slow and gradual formation of dust in CCSNe. Observationally, the trend exhibits a t (sup 2) behavior, exactly what is expected from an expanding optically-thick ejecta. In this case, the observed dust resides in the IR-thin "photosphere" of the ejecta, and constitutes only a fraction of the total dust mass. We therefore propose that dust formation proceeds very rapidly, condensing most available refractory elements within two years after the explosion. At early epochs, only a fraction of the dust emission escapes the ejecta accounting for the low observed dust mass. The ejecta's entire dust content is unveiled only a few decades after the explosion, with the gradual decrease in its IR opacity. Corroborating evidence for this picture includes the early depletions of refractory elements in the ejecta of SN1987A and the appearance of a silicate emission band around day 300 in SN2004et.

Dwek, Eli↗
NASA NTRS2019

Fine-Grained, Spinel-Rich Ca-Al-Rich Inclusions From The Reduced CV3 Chondrite Efremovka: A Genetic Link To Wark-Lovering Rims?

Fine-grained, spinel-rich Ca-Al-rich inclusions (FGIs) in carbonaceous chondrites, mostly CV3 chondrites, are interpreted as aggregates of nebular gas-solid condensates that escaped significant melting [1]. Multiple lines of evidence suggest a condensation origin for FGIs, including their layered structures and irregular shapes and the fine grain size of numerous spinel-cored nodules [e.g., 2,3], and the distinctive volatility-fractionated group II rare earth element patterns of bulk inclusions and their mineral constituents [e.g., 4,5]. The origin and nature of FGIs are poorly constrained because of their fine grain sizes and intimate intergrowths of refractory phases, combined with their susceptibility to secondary parent body alteration processes, making detailed mineralogical and petrologic characterizations difficult using scanning electron microscope (SEM) and electron microprobe techniques. In this study, we present preliminary transmission electron microscope (TEM) analyses of pristine FGIs from the reduced CV3 chondrite Efremovka in order to provide the detailed characterization of their micrometer- to nanometer-scale textures and chemical compositions. Our goals are to better understand the formation processes and conditions of FGIs in the early solar nebula and to explore their possible genetic relationship with other early-formed refractory inclusions and their rims.

Keller, L. P.↗
NASA NTRS2019

Complex Intergrowths of Non-Stoichiometric Defect-Structured Hibonite and Al-Rich Spinel in an Allende Ca-Al-Rich Inclusion

Hibonite is a primary ultra-refractory mineral occurring in many Ca-Al-rich inclusions (CAIs) and is predicted to condense as the second major phase from a cooling gas of solar composition. Our previous microstructural studies of hibonite in carbonaceous chondrites revealed its unique microstructures consisting of numerous defects that contain Mg-enriched, wider spinel blocks in stoichiometric hibonite. Han, J. et al. [2 items] demonstrated experimentally that defect-structured hibonites can grow easily in the presence of minor Mg and are kinetically more stable than equilibrium assemblages predicted by thermodynamic calculations. However, a thermo-dynamic vs. structural stability of defect-structured hibonite relative to other early-condensed Al-rich phases such as corundum, grossite, and spinel remains poorly constrained. Here, we present the results of atomic resolution TEM (Transmission Electron Microscopy) imaging of hibonite in a compact Type A CAI in the Allende CV3 chondrite in order to better understand the crystal structure and chemistry of defect-structured hibonite and its associated Al-rich phases, especially non-stoichiometric, Al-rich spinel, in the context of the formation of first refractory solids in the early solar nebula.

Han, J.↗
NASA NTRS2022

Atomic-Scale Structure and Non-Stoichiometry of Meteoritic Hibonite: A Transmission Electron Microscope Study

Hibonite (CaAl_12O_19) is a common refractory mineral in Ca-Al-rich inclusions (CAIs) in primitive meteorites. Transmission electron microscope (TEM) studies have identified enigmatic planar defects in different occurrences of hibonite in the Allende meteorite that give rise to strong streaking along c* in electron diffraction patterns. Atomic resolution high-angle annular dark-field (HAADF) imaging and energy-dispersive X-ray (EDX) analyses were used to determine the nature and origin of these planar features. HAADF images of hibonite grains reveal lamellar intergrowths of common 1.6 nm spacing, and less commonly 2.0 and 2.5 nm spacings, interspersed in stoichiometric hibonite showing 1.1 nm (002) spacing. Stoichiometric hibonite consists of alternating Ca-containing (“R”) and spinel-structured (“S”) blocks stacked in a sequence RS. In contrast, the 1.6 nm layers result from a doubled S block such that the stacking sequence is RSS, while in the widest defect observed, the stacking sequence is RSSSS. These intergrowths are epitaxial and have coherent, low-strain boundaries with the host hibonite Meteoritic hibonite shows common Ti and Mg substitution for Al in its structure. Atomic-resolution EDX maps of hibonite grains in the Allende CAI confirm the preferred site occupancy of Mg on tetragonal M3 sites in S blocks and of Ti on trigonal bipyramidal M2 and octahedral M4 sites in R blocks. Mg is highly concentrated, but Ti is absent in the planar defects where wider S blocks show Al-rich compositions compared to stoichiometric MgAl_2O_4 spinel. Therefore, Mg likely played the major role in the formation and metastability of planar defects in hibonite. Electron energy loss spectroscopy data from the Ti L_2,3 edge show the presence of mixed Ti oxidation states with ~ 15–20% of Ti as Ti^(3+) in hibonite, suggesting a direct substitution of Ti^(3+) ↔ Al^(3+) in hibonite. The remaining ~ 80–85% of Ti is present as Ti^(4+) and corresponding EDX analyses are consistent with the well-known coupled substitution 2Al^(3+) ↔ Ti^(4+) + Mg^(2+) being the major mechanism for Ti and Mg substitution in hibonite. The formation of planar defects in hibonite occurred during high-temperature nebular condensation or melting/crystallization processes. The occurrence of non-stoichiometric hibonite in the Allende CAI deviates from the mineral formation sequence predicted from equilibrium condensation models. Overall, our atomic resolution TEM observations signify non-equilibrium, kinetic-controlled crystal growth during the high-temperature formation of refractory solids in the early solar nebula.

hibonite↗
NASA NTRS2024

Chemical and Physical Properties of Cometary Dust

Cometary dust particles are best preserved remnants of the matter present at the onset of the formation of the Solar System. In Space missions, telescopic observations and laboratory analyses advanced the knowledge on the properties of cometary dust. the only samples certified with a cometary origin were returned by the Stardust space mission from comet 81P/Wild2. The “chondritic porous” (here called “chondritic anhydrous”) interplanetary dust particles (CA-IDPs) and micrometeorites (CP-MMs), and the ultracarbonaceous Antarctic MMs (UCAMMs) also show strong evidence for a cometary origin. The elemental composition of cometary dust is generally consistent with the chondritic (CI) composition, with the notable exception of elevated contents in carbon and nitrogen compared with CI. The organic matter of cometary dust is mixed with minor amounts of crystalline (at least 25% of the minerals) and amorphous mineral phases. The most abundant crystalline minerals are ferromagnesian silicates (olivine and low-Ca pyroxenes), but High-Ca pyroxenes, refractory minerals and Low Ni Fe sulfides are also present. The crystalline olivine and low-Ca pyroxene compositions can vary from their Mg-rich end-member (forsterite and enstatite) to relatively Fe-rich compositions. Refractory minerals as well as secondary minerals likeLIME (low-iron, Mn-enriched) olivines, unusual Fe sulfides or mineral aggregates of specific compositions like Kosmochloric high-Ca pyroxene and FeO-rich olivine - KOOL grains) are also found. The presence of carbonates in cometary dust is still debated, but a phyllosilicate-like phase was observed in a UCAMM. The abundance of pyroxene to olivine (in numbers) is larger than in primitive meteorites (e.g. the Px/Ol ratio is usually larger than 1). GEMS phases (glass with embedded metals and sulfides) are abundant in cometary dust, although not systematically found. Some of the organic matter present in cometary dust particle resembles the insoluble organic matter (IOM) present in primitive meteorites, but amorphous carbon and exotic (e.g. N-rich) organic phases are also present. The hydrogen isotopic composition of cometary dust particles (in the organic matter) is usually rich in deuterium, tracing a formation at very low temperatures, either in the protosolar cloud or in the outer regions of the protoplanetary disk. The presolar dust concentration in cometary dust can reach about 1%, which is the most elevated value observed in extraterrestrial samples. The size distribution of cometary dust in comet trails is well represented by a power-law distribution (differential size distribution) with a mean power index N typically ranging from -3 to -4. Polarimetric and light scattering studies of cometary dust suggest mixtures of porous agglomerates of sub-micrometer minerals with organic matter, which is compatible with the in situ analyses of 67P/Churyumov-Gerasimenko by MIDAS (Rosetta) and with the studies of it Stardust samples, CA-IDPs, CP-MMs and UCAMMs. Cometary dust particles have low tensile strength, and low density.

C. Engrand↗
NASA NTRSDate not supplied

Prometheus and Constellation Materials Research and Testing Overview

Outline - New Technologies and New Materials meet Flight Program - Reactor Materials Selection - Material Radiation Resistance - Testing in four different radiation environments - Superalloy Creep Testing - Superalloy-Refractory Alloy Joining - Superalloy, Stainless Steel, Copper Brazing - Superalloy-Refractory Cross Contamination - Na and NaK Compatibility - Radiator Panel Materials Selection

nuclear power↗
NASA NTRS2023

Galvanic Protected Anode Materials for Molten Regolith Electrolysis

This effort aimed to explore the use of refractory alloys as long-lifetime electrode materials for use in a molten regolith electrolysis (MRE) reactor, a technology that can produce oxygen (O2) from regolith. To find a material capable of withstanding the high temperatures and corrosive nature of molten regolith, first-principles thermodynamic calculations were performed on platinum group metals in the presence of iron (Fe) and silicon (Si) to determine favorable compositions for resisting unwanted secondary phases that could form on the surface of the material. As a result of these first-principles calculations, the kinetic properties of elements such as aluminum (Al), Fe, and Si can be more easily derived, which would provide insight into the longevity of such a material when used in an MRE reactor. The effort funded by this CIF project mapped the entire phase diagram of platinum group metals, which is beneficial not only to MRE where high temperatures and molten material are present, but also aerospace applications like turbine materials, terrestrial metal processing techniques, and energy storage applications. This project narrowed a broad spectrum of refractory metals down to a small list of alloys that would be able to survive not only the high temperatures of an MRE reactor, but also the thermodynamic forces that would cause inferior alloys to form secondary phases, which would ultimately consume the electrodes of the reactor. This research needs to be followed up with experimental demonstrations of these alloys in an MRE environment.

Kevin Grossman↗
NASA NTRSDate not supplied

Mineralogical Analysis of Calcium-Aluminum-Rich Inclusions Provides Insight Into Post-Formation Processes

Introduction: Calcium-aluminum inclusions (CAIs) are cm- to mm-sized intergrowths of refractory phases found in chondritic meteorites [1]. Their mineral compositions closely match the compositions of the solids thought to condense from an extremely hot (>1500K) gas with a bulk solar composition [2-4], suggesting that CAIs were the earliest solids within the Solar System [2-4]. These inclusions provide invaluable insights into the conditions and dynamics of the early Solar System. CAIs must be transported from their formation region near the protosun to the chondrite parent-body accretion region. The nature of their journey could affect how, when, and where the secondary processes recorded in these CAIs occurred [4]. Did these secondary processes occur in the solar nebula or during accretion with the parent body, or both? How were the CAIs affected by varying thermochemical processes? To better answer these questions, we have undertaken an in-depth, textural study of the secondary alteration of select CAI samples. Methods: We chose three CAIs that experienced a range of post-formation processing to gain better understanding of secondary alteration based on previous preliminary examination [5]. Representative CAIs were chosen from NWA 5508 (CV3), NWA 12772 (CV3), and Coolidge (CL4) carbonaceous chondrites. We used scanning electron microscopy (SEM) and electron backscatter diffraction (EBSD) techniques for detailed chemical, mineralogical, and textural analysis of the CAIs. Backscattered electron (BSE) images and X-ray elemental maps were taken of Coolidge and NWA 5508 using the Lunar and Planetary Institute (LPI) Phenom SEM. The JEOL 7900F SEM at NASA Johnson Space Center (JSC) was used to obtain energy dispersive spectroscopy (EDS) chemical maps of all samples. High resolution EBSD analysis identified the mineral phases and textures, providing key information on their nature. Based on the SEM and EBSD data, minerals of interest were selected for quantitative chemical electron probe micro-analysis (EPMA) using the JEOL JXA-8530F at NASA JSC. Results and Discussion: The EDS maps show that the NWA 5508 and NWA 12772 CAIs designated “Saguaro” and “Hoopoe” respectively [5] are enriched in calcium while the Coolidge CAI designated “Cottonwood” is aluminum and magnesium rich. Saguaro. A ~1.5cm diameter igneous Type B CAI with a rounded shape. The dominant phases are melilite, spinel, and Al-Ti pyroxene with minor anorthite. Spinel is subhedral and occurs in clusters. Some of these clusters have a circular geometry which encloses other minerals, known as a palisade structure [6] (Fig. 1). Some palisades form near perfect circles while others are more irregular in shape. Melilite in Saguaro ranges in size from coarse (>250m) to fine-grained (5-7m) and forms intergrown laths. A third of the melilite grains exhibit simple twinning about their <001> axis. The spinel palisades and twinned melilite in Saguaro suggest an igneous history, and the lack of secondary minerals suggests minimal aqueous alteration. At some point in time after the initial condensation of the minerals and formation of the inclusion, the sample was remelted and quickly solidified. The formation of the palisades is still heavily debated. One hypothesis is that the palisades are the rims of smaller CAIs that accreted early on, essentially acting as xenoliths within the larger CAIs [7]. Another hypothesis suggests an igneous origin for palisade structures [6-8] wherein the melt traps gas bubbles, and the spinel nucleates on the surface of this bubble. Based on the WDS spot analyses of 41 melilite grains using EPMA, the data suggest that the composition inside and outside the palisades is nearly identical. This finding indicates that these palisades are likely not exogenous but rather formed from melt-vapor reactions. Our results are consistent with studies by Simon and Grossman,1997 [6] and Zhang et al. (2019) [8]. Hoopoe. A ~0.5cm compact Type A CAI with an irregular shape. The dominant mineral phases are melilite, spinel, and hibonite with minor amounts of anorthite, augite, and perovskite. The melilite ranges in size from ~500 to 50µm. The larger melilite grains have simple twinning along the <001> axis like melilite in Saguaro. Melilite in Hoopoe exhibits crystal-plastic strain with misorientation dominantly about the <010> and <110> axes. Spinel shows subhedral to euhedral morphology and appears in clusters. Hibonite grains are similar to spinel in habit and size but show more plastic strain. The two minerals are often found together with one appearing to replace the other. Perovskite appears in fine grained recrystallized regions alongside fine augite and spinel. The abundant strain and deformation features in the melilite and hibonite suggest that Hoopoe experienced shock. This shock could have occurred in the nebula [9] or from an impact of another body on the parent body asteroid. The appearance of fine-grained (<10m) areas of augite, perovskite, and spinel in the dominantly coarse-grained inclusion suggest recrystallization, possibly due to the sudden increase in pressure and temperature. Cottonwood. This ~0.5cm CAI exhibits distinct mineralogy and textures suggesting a high degree of alteration. It is irregular in shape. The dominant mineral phases are spinel and anorthite with minor amounts of augite and rutile. The two main texture types can be seen in Fig. 2. The first type consists of coarse euhedral to subhedral spinel and anorthite. The second includes fine grained spinel, anorthite, rutile, and iron sulfides. Within these fine-grained regions, the anorthite grains are clustered into domains exhibiting the same crystallographic orientation. Rutile exclusively occurs with fine anorthite indicating a potential relationship between the two. Cottonwood has a clear and unbroken Wark-Lovering [10] rim (Fig. 2) on one side that consists of a sequence of spinel followed by anorthite and an outer layer of augite. The abundance of the fine-grained regions containing iron oxides and iron sulfides, secondary phases such as rutile, and oriented anorthite grains is evidence for recrystallization associated with a high degree of thermal metamorphism. The EPMA analyses on both coarse- and fine-grained spinel show that the fine spinel grains are more enriched in Cr (1-2 wt. %) than their coarse counterparts (0.1-0.5 wt. %). The data suggest thermal metamorphism drove chemical exchange of the previously refractory inclusion, introducing chromium and iron as well as sulfur, which is moderately volatile. Conclusions: The three CAIs analyzed record distinct secondary nebular and parent body processes. Saguaro melted in the nebula as seen by the twinned melilite and spinel palisades. Hoopoe experienced intense shock which deformed its melilite and recrystallized perovskite, augite, and spinel in fine-grained regions. Cottonwood shows evidence of recrystallization and chemical changes consistent with thermal metamorphism occurring after accretion into the parent-body.

V E Burnette↗
NASA NTRSDate not supplied

Anhydrous Primary Minerals in Ryugu, Ivuna, and Bennu

Samples returned from asteroid Ryugu are chemically and mineralogically similar to CI chondrites [e.g., 1–3]. Both are predominantly composed of low-temperature aqueously formed secondary minerals, whereas high-temperature anhydrous primary minerals, such as olivine, low-Ca pyroxene, spinel, and hibonite, are rarely present. Using secondary ion mass spectrometry (SIMS; Cameca ims-1280HR at Hokkaido University), we performed O [4] and Al–Mg [5] isotope measurements of anhydrous primary minerals in samples of Ryugu and the Ivuna CI chondrite to constrain their origin.Anhydrous primary minerals in our samples of Ryugu and Ivuna occur mostly as monomineralic isolated grains embedded in hydrated matrix. Their O-isotope compositions are distributed along the slope-1 line on the O three-isotope diagram and range from Δ17O ~ –23 to 0‰. Mg-Al spinel grains are 16O-rich (Δ17O ~ –23‰). Low-Ca pyroxene grains are 16O-poor (Δ17O ~ –5‰). Olivine grains show a bimodal distribution of O-isotope composition:10 of 34 grains measured are 16O-rich (Δ17O ~ –23‰) and 24 grains are 16O-poor (Δ17O ~ –7 to 0‰). We found refractory inclusions composed of Mg-Al spinel and hibonite, one from Ryugu and one from Ivuna. Also, in Ivuna, we found an amoeboid olivine aggregate ( AOA) composed of olivine, diopside, anorthite, and Mg-Al spinel and an inclusion composed of olivine and Mg-Al spinel. The minerals in all of these inclusions are 16O-rich (Δ17O ~ –24‰).The 16O-rich grains and inclusions are mineralogically and O-isotopically similar to calcium-aluminum–rich inclusions (CAIs) and AOAs reported in other carbonaceous chondrites [6, 7]. In addition, the initial 26Al/27Al ratios of the two spinel-hibonite inclusions are inferred as ~4.4 × 10–5, also similar to most CAIs in carbonaceous chondrites [6, 8]. The range of Δ17O values for the 16O-poor olivine and low-Ca pyroxene grains is consistent withthat of these minerals in chondrules in most carbonaceous chondrites [9]. Moreover, the most frequent Δ17O value (–6‰) for Mg-rich (Mg# > 97) olivine grains is identical to those for chondrules. Although CI chondrites and Ryugu samples are devoid of chondrules, the 16O-poor grains most likely represent fragments of chondrule-like objects. The presence of both 16O-poor chondrule-like and 16O-rich refractory inclusion–like minerals in Ryugu and Ivuna suggests that some of their building blocks are similar to those of other carbonaceous chondrite groups. They both probably formed in the inner solar protoplanetary disk and were subsequently transported outward.Preliminary data for petrography of asteroid Bennu samples and chemical and isotopic compositions of theiranhydrous primary minerals will also be presented in the meeting.

N Kawasaki↗
DOE OSTI2012

Sulfur tolerant highly durable CO.sub.2 sorbents

A sorbent for the capture of carbon dioxide from a gas stream is provided, the sorbent containing calcium oxide (CaO) and at least one refractory dopant having a Tammann temperature greater than about 530.degree. C., wherein the refractory dopant enhances resistance to sintering, thereby conserving performance of the sorbent at temperatures of at least about 530.degree. C. Also provided are doped CaO sorbents for the capture of carbon dioxide in the presence of SO.sub.2.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2012

Automating the Coupling of ORIGEN with GADRAS via the Fallout Analysis Tool for National Technical Nuclear Forensics

Nuclear forensic teams will be deployed to collect and evaluate fallout samples on the ground in the scenario of a low-yield nuclear detonation in a heavily populated area. Quick non-destructive methods of predicting the quality of the sample before it is analyzed in detail are essential for efficient post-event collections. In this work, the process of exporting Defense Land Fallout Interpretive Code (DELFIC) results into Gamma Detector Response and Analysis Software (GADRAS) has been automated within the Fallout Analysis Tool. This coupling allows for the simulation of detector responses to fallout samples with varying degrees of fractionation. The degree to which the samples are fractionated depends on the location of the samples in the fallout field. In the following study, this phenomenon is examined, as its understanding is important to the investigation of debris distribution. The simulated detector spectra from GADRAS can be used to compare peak ratios of volatile-refractory isotope pairs in order to determine the degree of fractionation. Simulated fractionated fallout samples from DELFIC for a 10 kt, pure 235U fission surface burst were modeled for distances ranging to 256 km out from ground zero, and for times up to 1 week from detonation. The fractionation ratios, also known as r values, from isotope concentrations, photon lines and peak areas of four volatile-refractory pairs were calculated and compared. Fractionation prediction via the peak areas method was evaluated for each pair by comparing the results with the simulated radionuclide inventory.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗