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NASA NTRS2014

Texture-Induced Anisotropy in an Inconel 718 Alloy Deposited Using Electron Beam Freeform Fabrication

A test block of Inconel (IN) 718 was fabricated using electron beam freeform fabrication (EBF(sup 3)) to examine how the EBF(sup 3) deposition process affects the microstructure, crystallographic texture, and mechanical properties of IN 718. Tests revealed significant anisotropy in the elastic modulus for the as-deposited IN 718. Subsequent tests were conducted on specimens subjected to a heat treatment designed to decrease the level of anisotropy. Electron backscatter diffraction (EBSD) was used to characterize crystallographic texture in the as-deposited and heat treated conditions. The anisotropy in the as-deposited condition was strongly affected by texture as evidenced by its dependence on orientation relative to the deposition direction. Heat treatment resulted in a significant improvement in modulus of the EBF(sup 3) product to a level nearly equivalent to that for wrought IN 718 with reduced anisotropy; reduction in texture through recrystallization; and production of a more homogeneous microstructure.

Tayon, W.↗

NASA NTRS2015

Na, K-Rich Rim Around a Chondrule in Unequilibrated Ordinary Chondrite Lew 86018 (L3.1)

Ordinary chondrites represent the most abundant early Solar system extra-terrestrial (approximately 85% abundance) material available for laboratory studies and expectedly record the most extensive range of alterations effects from unmetamorphosed chondritic material to the highest temperatures of thermal metamorphism. The least metamorphosed chondrites belonging to petrologic type 3, the so called unequili-brated ordinary chondrites (UOCs), provide insights into alteration that happened during the primeval, ear-liest stage of Solar system formation. The higher grade petrologic types 4-6 ordinary chondrites on the other hand document up to near textural equilibrium (in type 6) extensive thermal metamorphism consisting of minerals and phases providing evidence of equilibration of heterogeneous mineral composition, solid-state recrystallization. Despite being the most abundant, the effect of alteration is less explicitly understood in ordinary chondrites (even less in UOCs) compared to other groups (e.g. CV, CO, CR). Additionally, the relationship between metasomatism (also referred as aqueous alteration or fluid-assisted metamorphism) and metamorphism (primarily thermal driven) has not been studied and alterations in the ordinary chondrites have been considered to have occurred in absence of fluids in general. Despite this conventional view, UOCs of lowest grades (3.0-3.2) show some evidence of low temperature (approximately 200 C), fluid assisted metamorphism in the form of the presence of phyllosilicates, ferroan olivine, and magnetites in their matrices and occasionally in chondrules. Here, we present petrographic and mineralogical studies of UOC, Lewis Hills (LEW) 86018 to further our understanding of the extent and relative importance of metasomatism and/or metamorphism in UOCs.

Mishra, R. K.↗

NASA NTRS2016

An Amoeboid Olivine Aggregate in LEW 85300

Amoeboid Olivine aggregates (AOAs) are irregularly shaped objects commonly observed in carbonaceous chondrites. Because they are composed of fine-grained olivine and Ca-Al-rich minerals, they are sensitive indicators for nebular process and parent body alteration of their parent bodies. Recently an AOA was found in a carbonaceous clast in polymict eucrite LEW 85300. The bulk major element composition of the clast matrix in LEW 85300 suggests a relation to CM, CO and CV chondrites, whereas bulk clast trace and major element compositions do not match any carbonaceous chondrite, suggesting they have a unique origin. Here we characterize the mineralogy of AOA in LEW 85300 and discuss the origin of the carbonaceous clasts. Results and Discussion: The AOA is located in an impact melt vein. Half of the aggregate shows recrystallization textures (euhedral pyroxene and molten metal/FeS) due to impact melting, but the remaining part preserves the original texture. The AOA is composed of olivine, FeS and Mg,Al-phyllosilicate. Individual olivine grains measure 1-8 microns, with Fe-rich rims, probably due to impact heating. Olivines in the AOA are highly forsteritic (Fo95-99), indicating that the AOA escaped thermal metamorphism [4]. Although no LIME (Low-Fe, Mn-Enriched) olivine is observed, forsterite composition and the coexistence of Mg,Al-phyllosilicate suggest that the AOA is similar to those in the Bali-type oxidized CV (CVoxB) and CR chondrites. However, it should be noted that fayalitic olivine, which commonly occurs in CVoxB AOA, is not observed in this AOA. Also, the smaller grain size (<8 microns) of olivine suggests they may be related to CM or CO chondrites. Therefore, we cannot exclude the possibility that the AOA originated from a unique carbonaceous chondrite.

Komatsu, M. D.↗

NASA NTRS2016

Parallel Grand Canonical Monte Carlo (ParaGrandMC) Simulation Code

This report provides an overview of the Parallel Grand Canonical Monte Carlo (ParaGrandMC) simulation code. This is a highly scalable parallel FORTRAN code for simulating the thermodynamic evolution of metal alloy systems at the atomic level, and predicting the thermodynamic state, phase diagram, chemical composition and mechanical properties. The code is designed to simulate multi-component alloy systems, predict solid-state phase transformations such as austenite-martensite transformations, precipitate formation, recrystallization, capillary effects at interfaces, surface absorption, etc., which can aid the design of novel metallic alloys. While the software is mainly tailored for modeling metal alloys, it can also be used for other types of solid-state systems, and to some degree for liquid or gaseous systems, including multiphase systems forming solid-liquid-gas interfaces.

Vesselin I Yamakov↗

NASA NTRS2017

Clast Selection and Metallographic Cooling Rates: Initial Results on Type 1A and 2A Mesosiderites

We initiated a comprehensive study on selected clasts and metal of mesosiderites using SEM, electron microprobe and the complete suite of noble gases. Here we report initial results on the petrography of selected clasts and metallographic cooling rates using the central Ni method used in sev-eral publications. We focus on the approach of selecting grains in least recrystallized mesosiderites. Hence, especially (lithic) clasts in type 1A, 1B, 2A and 2B are the first choice. They provide highest primitive-ness and least annealing/metamorphism. All grains selected should be in close proximity to each other. Lithic clasts in mesosiderites are of high interest be-cause of their igneous texture and similarity to eucrites and howardite petrography. We find pyrox-enes (px) and plagioclase (plag) attached to each other which implies a common formation history. It will be interesting to see differences and similarities in their noble gas inventory (CRE ages, trapped components and closure temperature). In addition, we will investi-gate variations of the lithic clasts toward similar grains in the thick sections which are not igneous. Plag grains are the best bases for noble gas measurements con-cerning He to Ar and Ar-Ar dating since it delivers im-portant target elements. We focus on plag grains in close contact to olivine (olv) / px grains to assess weth-er both grains show noble gas patterns being similar or different. Phosphate grains are suitable for Kr and Xe measurements since they yield REE abundances (tar-get elements).

Mesosiderites↗

NASA NTRS2018

Primitive Oxygen-, Nitrogen-, and Organic-Rich Vein Preserved in a Xenolith Hosted in the Metamorphosed Carancas Meteorite

Primitive xenolithic CI-like carbonaceous (C) clasts are sometimes hosted within meteorites of a different origin (ordinary chondrite, ureilite, howardite, and eucrite). These xenoliths contain aggregates of macromolecular carbon (MMC), which are often present as discrete grains and exhibit a wide range of structural order and chemical compositions. The Carancas meteorite is a H4-5 that impacted south of Lake Titicaca, Peru in 2007. While the meteorite exhibits extensive recrystallization of the matrix indicating metamorphism, it contains dark, CI-like clasts that show no evidence of heating. Similar to other xenolithic clasts, the examined C clast of Carancas contains MMC, which however exists in the form of a vein-like structure dissimilar to the typical occurrence of MMC in meteorites. We investigated the organic and isotopic compositions of the organic-rich vein with C,N,O-X-ray absorption near-edge structure (XANES), Raman spectroscopy, and NanoSIMS, in order to constrain its possible origin.

Chan, Q. H. S.↗

NASA NTRS2018

Impact of Powder Variability on the Microstructure and Mechanical Behavior of Selective Laser Melted Alloy 718

Powder-bed additive manufacturing processes use fine powders to build parts layer-by-layer. Alloy 718 powder feedstocks for selective laser melting (SLM) additive manufacturing are produced commercially by both gas and rotary atomization and are available typically in the 10-45 or 15-45 microns size ranges. A comprehensive investigation was conducted to understand the impact of powder variability on the microstructure and mechanical behavior of SLM 718 heat treated to Aerospace Material Specification (AMS) 5664. This study included sixteen virgin powders and three once-recycled powders within the 10-45 and 15-45 microns size ranges that were obtained from seven direct source suppliers and one reseller. Although alike as highly regular spheroids, these powders showed distinct differences in composition (especially Al, C and N contents), particle size distributions, and powder features such as degree of agglomeration, fusion and surface roughness. Compositional differences expectedly had the strongest impact on microstructure. High N and C contents formed TiN-nitrides and/or (Nb,Ti,Mo)-C carbides on the grain boundaries, prevented recrystallization during heat treatment, and resulted in retained (001)-scalloped shaped grains that ranged from 19 to 41 microns in average size. In the absence of this particle pinning, the average grain size of the heat treated SLM 718 ranged from 51 microns to 90 microns. Room temperature tensile and high cycle fatigue (HCF) testing compared as-fabricated (AF) and low stress ground (LSG) surface conditions. Tensile testing revealed consistent behavior between the two surface conditions and amongst the powder lots. The finer grained SLM 718 builds displayed the lowest tensile properties. A SLM 718 build fabricated from a powder with eight times lower C content showed statistically better tensile properties presumably due to enhanced coarsening of (delta)-Ni3Nb precipitates. The specimens from once-recycled powders had slightly higher tensile strengths and slightly higher ductility compared to their virgin equivalents; once-recycling also did not substantially degrade the mean HCF life. The LSG fatigue lives agreed with conventionally manufactured 718 data, while AF lives exhibited a knock-down due to surface roughness. The fatigue lives of AF specimens were statistically equivalent across powder lots except for one and failures typically initiated at stress concentrators associated with SLM surface asperities. Fatigue testing of low stress ground specimens result in both transgranular and within facet crack initiations. More than half of the cracks initiated from these facets for the machined condition; however, these facets appeared to be within grains that were larger-than-average in size. A nitrogen-atomized powder with fine prior particles of TiN-nitrides and M(Ti,Nb,Mo)C carbides from atomization on powder surfaces resulted in the best fatigue performance with segregation of these particles to the SLM 718 grain boundaries leading to higher resistance to early-stage crack propagation. Typically the fine-grained builds with minor phases along the grain boundaries did not perform well in fatigue, whereas a larger-grain build with lower carbon content and coarser delta-Ni3Nb precipitates showed the next best HCF response. Further details of the build microstructure and its impact on tensile and fatigue behavior was considered.

laser deposition↗

NASA NTRS2018

Mineralogical Study of a White Clast from Murchison (CM2): Comparison with R-Chondrites

R-chondrites share some properties with ordinary chondrites (OC) and carbonaceous chondrites (CC). The proportions of the textural types of chondrule from R chondrites and their FeO/(FeO+MgO) ratios are similar to those of OC, but the high matrix abundance in R chondrites more closely resembles that of CC (matrix abundances: OC ~12 vol% vs. CC 34->60 vol%;). In this study, we characteristize the mineralogy of a white clast from Murchison (CM2), which was earlier considered to be a R-chondrite. First, all the petrographic and mineralogical characteristics will be described and compared with those of R-chondrites. Finally, all data will be considered in order to test, whether this clast is a real R-chondrite or a unique recrystallized chondrite?

Kerraouch, I.↗

NASA NTRS2018

Novel Shock Microstructures in Accessory Minerals from the Haughton Dome, Devon Island, Nunavut, Canada

The 23 km-diameter, ca. 24 Ma Haughton Dome impact structure in the Canadian Arctic on Devon Island, Nunavut (89deg41′W, 75deg22′N) occurred within a two layered target composed of a shallowly-dipping ~1700 m thick succession of Paleozoic limestones and evaporates overlying ca.1.9 Ga high grade gneisses [1, 2]. Within the structure a well preserved impact melt bearing breccia unit contains a variety of shocked clasts from the pre-impact sediments and basement gneisses [3]. Due to their high level of preservation a variety of studies have been undertaken on the clast population of the melt bearing breccia, including characterization of shock within the accessory minerals of the basement lithologies [4, 5]. This study presents high resolution electron backscatter diffraction (EBSD) microstructural data for zircon and monazite from historic samples of the basement gneiss, in which bulk shock pressures have been previously constrained based on major phases [4, 6]. Shocked zircon and monazite grains have been investigated from shock stage 1b (sample 72110), 2 (7273) and 3 (7192, Dig-9) [4, 6]. At lower shock levels zircon displays planar microstructures consistent with mechanical shock {112} twin formation [7] and deviatoric transformation to the high pressure polymorph reidite [8]. Zircon grains from shock stage three show a more chaotic microstructure with multiple orientations of tightly spaced sets of reidite that are variably recrystallized to zircon neoblasts. Monazite from lower shock stages contains a number of mechanical twin orientations that are indicative of shock deformation [9]. At higher shock pressures a lath like structure of interlocking twin orientations has been identified. This microstructure is suggestive of a reversion transformation from a high pressure polymorph [10] and is the first evidence for the transformation of monazite during shock.

Erickson, Timmons M.↗

NASA NTRS2019

Unravelling Complex Geologic Histories Using U–Pb and Trace Element Systematics of Titanite

Unravelling the spatio-temporal evolution of orogenic terranes requires a comprehensive understanding of the duration and extent of metamorphic events and hydrothermal alteration. Commonly used minerals such as zircon and monazite may not fully record geological histories in complex tectonic settings because their elemental constituents do not react under many metamorphic and metasomatic conditions. Here, we complement the current geochronological record of the Capricorn Orogen, Western Australia, with titanite U–Pb geochronology and geochemistry of felsic intrusive rocks to draw conclusions about the use of titanite in understanding the evolution of orogenic terranes. Because titanite usually incorporates common-Pb and may be variably reset by multiple metamorphic and hydrothermal events, a workflow is provided here for the systematic and robust interpretation of titanite U-Pb data. The addition of trace element data in titanite is particularly effective for differentiating whether a grain is igneous, recrystallized or metamorphic. We have developed several petrogenetic indices to differentiate these three types of titanite using Zr-in-titanite temperature, Th/U, Th/Pb, Al/(Al + Fe), light to heavy rare earth element ratio, and Eu anomalies. The addition of trace element geochemistry can also highlight anomalously radiogenic (sup 207)Pb/(sup 206)Pb reservoirs. Utilization of our workflow in the Capricorn Orogen reveals that titanite ages from the same samples as published zircon U–Pb data range from coeval to several hundreds of Myr of age difference between the two minerals. Titanite geochronology and trace element geochemistry indicates ~20 Myr of previously unrecognized prolonged cooling for the Capricorn Orogeny to ca. 1750 Ma. The spatial extent of the ca. 1210–1170 Ma part of the Mutherbukin Tectonic Event is also broadened significantly farther north and south than previously recognized. Incorporating titanite geochronology and trace geochemistry with more commonly used techniques (e.g., zircon and monazite petrochronology) extends our ability to resolve the complete history of large-scale orogenic terranes.

Hugo K. H. Olierook↗

NASA NTRS2020

Petrology of Chondrule Rims in Yamato-791498 and Asuka-881828, the Least-Altered CR Chondrites in the Japanese NIPR Collection

CR chondrites are a group of car-bonaceous chondrites with well-preserved records of formation of their components in the solar nebula. The CR chondrites have undergone a wide range of aqueous alteration from nearly anhydrous (CR2.8 or CR3.0) to extensive recrystallization of primary minerals, including replacement of coarse-grained silicates in chondrules (CR2.0). At the same time, CRs have experienced only minor thermal metamorphism except for rare CR6 samples. Identifying minimally altered CR chondrites is a priority because they preserve (1) relatively pristine records of the solar nebula and (2) minerals and textures at the beginning stages of aqueous alteration. Here we report the petrologic characteristics of Y-791498 and A-881828 as the least aqueously altered CR chondrites in the Japanese NIPR meteorite collection. Previous studies have shown that fine-grained rims on chondrules are indicators of incipient alteration of primitive CR chondrites, there-fore we focus on rims around chondrules in the two meteorites.

Komatsu, M.↗

NASA NTRSDate not supplied

Deciphering Extreme Mineral Records; Microstructural Phase Heritage of Shocked Materials

High-pressure minerals such as coesite, stishovite, and reidite are often used as indicators of shock metamorphism. However, high-pressure and high-temperature phases are metastable at ambient conditions and, therefore, often revert to a more energetically favorable phase. During solid-state transformations, the crystallographic orientations of the stable polymorph are controlled by the transformation pathway from the parent. Microstructural orientation analysis using electron backscatter diffraction (EBSD) of the stable phase can reveal systematic intercrystalline orientation relationships (OR) diagnostic of solid-state transformations from these high-pressure or high-temperature polymorph phases (Cayron et al., 2006). Knowledge of polymorph stability fields for a given system can thus be used to infer minimum shock P and/or T conditions that rocks have experienced, which are otherwise unavailable using traditional thermobarometers such as element partition coefficients. Using orientation relationships to infer the former presence of mineral phases has been termed microstructural “phase heritage”, and has successfully been used to probe for evidence of extreme pressures and temperatures resulting from hypervelocity impacts. The reconstruction of polymorphs of ZrSiO4 (zircon, reidite) and ZrO2 (baddeleyite) have further elucidated the behavior of these phases under hypervelocity impact conditions (Timms et al., 2017a; White et al., 2018), and OR analysis of shocked monazite has identified a previously unrecognized tetragonal high-P polymorph (Erickson et al., 2019). Zircon will convert to the low tetragonal polymorph reidite at shock stresses above ~21 GPa. However, upon decompression at temperatures above 1200 °C reidite will revert to zircon (Kusaba et al., 1985). Recrystallized zircon neoblasts encased in impact melt often show systematic misorientation relationships of 90° about <110> indicative of reversion from the reidite (Fig. 1), and preserving cryptic evidence of the high-P history that is often erased by the post shock thermal spike (Cavosie et al., 2016). Microstructural OR analysis of a dissociated zircon corona composed of baddeleyite (monoclinic-ZrO2) has identified the former presence of cubic zirconia within impact melt glass from the Mistastin Lake impact structure, Labrador, CA. Based on stability fields in the ZrO2-SiO2 binary phase diagram, cubic zirconia records thermal conditions in excess of 2370 °C at ambient P, indicating that the Mistastin impact melt is the hottest rock identified on Earth’s surface (Timms et al., 2017b). Shock-deformed monazite (monoclinic La,Ce,ThPO4) containing lamellae comprised of interlocking laths has been identified from the Haughton Dome impact structure, Nunavut, Canada and Nördlinger-Ries Crater, southern Germany. The lath-structured lamellae are composed of four systematic orientation variants, which OR analyses indicate originate from a tetragonal parent whereby the [010]monoclinic aligns with either [100] or [010]tetragonal (Erickson et al., 2019). These results highlight utility of microstructural phase heritage analyses for the identification of unstable high-P or high-T polymorphs that uniquely record the extremely transient shock conditions produced by hypervelocity impacts.

Timmons Erickson↗

NASA NTRS2022

Parallel Grand-Canonical Monte Carlo (ParaGrandMC) User’s Manual Version 2.0

This manual describes the commands and command line options for the Parallel Grand Canonical Monte Carlo version 2.0 (ParaGrandMC.2.0) simulation code. This is a highly scalable parallel FORTRAN 2003 code for simulating the thermodynamic evolution of materials at the atomic level, and predicting their thermodynamic state, phase diagram, chemical composition and mechanical properties. The code is specifically designed to simulate multi-component alloy systems, predict solid-state phase transformations such as austenite-martensite transformations, precipitate formation, recrystallization, capillary effects at interfaces, surface absorption, etc., which can aid the design of novel metallic alloys. While the software is mainly tailored for modeling metal alloys, it can also be used for other types of solid-state systems, and to some degree for liquid or gaseous systems, including multiphase systems forming solid-liquid-gas interfaces. In addition to performing Monte Carlo (MC) simulations, the code can also perform Molecular Dynamics (MD) and Langevin Dynamics (LD) simulations, which can be combined and interchanged with MC for faster and more efficient system evolution. A detailed description of the MC part of the code is provided in the NASA ParaGrandMC report: NASA/CR–2016-219202; http://www.sti.nasa.gov.

High performance computing↗

NASA NTRSDate not supplied

Tin-Essako 001: A Metal-Rich Ureilite?

Introduction: Metal-rich achondrites include a variety of types, and likely have a variety of origins. Models range from gravitational mixing at the core-mantle boundaries of differentatiated asteroids, to complex impact mixing scenarios. We describe a new type of metal-rich achondrite that might be the first metal-rich ureilite. Sample: Tin-Essako (TE) 001 (~4.3 g) was found in Mali in 2020 and purchased by Jay Piatek in 2021. It was classified as a metal-rich ungrouped achondrite, with olivine and oxygen isotope (d18O=8.2810‰, d17O=3.718‰, avg. 3) compositions suggesting affinity to ureilites [1]. We studied one polished section (~187.7 mm2) of TE 001. Petrography: TE 001 consists of ~60% metal and 40% silicates, heterogeneously distributed. The metal is largely fresh, but iron oxides (presumably terrestrial) occur along one edge and in some patches and veins in the interior. The silicates are dominantly olivine (≥90%), with melt-textured areas of plagioclase + Si-rich glass. Minor phases include chromite and carbon. Olivine occurs as rounded grains (up to ~2.5 mm) in metal, commonly with rims of melt-textured plagioclase + glass. Olivine also occurs in more massive areas having a “honeycomb” texture, with rounded olivine “cells” surrounded by an interstitial network of reduced olivine riddled with tiny metal grains, plus melt-textured plagioclase + Si-rich glass. Chromite occurs as subhedral to rounded grains; smaller grains (30-250 mm) are included in olivine and a few larger grains (400-500 mm) are isolated within metal. A carbon phase occurs as lacy-textured rims around olivine grains in metal, or small patches within metal. Mineral Compositions: The olivine (excluding interstitial areas) is Fo 73.9±0.5, with 0.25±0.02 wt.% CaO, 0.31±0.01 wt% Cr2O3, 0.01 wt.% NiO, and molar Fe/Mn=49.8±2.2 (53 analyses). Olivine in interstitial areas has Fo up to at least 91. Smaller chromite grains have Fe# (molar Fe/[Fe+Mg]) = 0.54±0.01, Cr# (molar Cr/[Cr+Al]) = 0.52±0.01, 0.52±0.02 wt.% V2O3 and 0.21±0.04 wt% ZnO (28 analyses). One larger grain is zoned from Fe# = 0.45, Cr# =0.52 to Fe# = 0.40, Cr# =0.57, and contains thin Al-rich lamellae not resolved by EMPA. One irregularly shaped patch of chromite included in olivine has Fe# =0.26 and contains no ZnO. Plagioclase laths are An ~53-60, with ≤0.01 wt.% K2O. Glass contains 75-76 wt% SiO2 and ~16 wt% Al2O3. The metal contains 5.2±0.2 wt% Ni, 0.46±0.02 wt.% Co, and 0.01±0.01 wt.% Cr, with Si and P below detection (168 analyses). Discussion: The olivine + chromite assemblage in TE 001 is similar to the most ferroan ureilites (Fo ~75-79 [2]), as are the oxygen isotopes [1]. The presence of a carbon phase supports this, although the identity of this phase (graphite as in ureilites?) remains to be determined. The “honeycomb” textured areas, in particular, the presence of olivine “reduction rims,” resemble shock-smelted olivine areas in ureilites [3], but interstitial melt-textured plagioclase laths + glass like those in TE 001 have not been reported in such (or any) ureilites. Olivine in TE 001 is marginally more ferroan than in the most FeO-rich ureilite, with Fe-Mg-Mn composition offset from the trend of olivine + low-Ca pyroxene ureilites similar to augite-bearing ureilites [4]. CaO and Cr2O3 contents are in the range of those in ureilite olivine [ ] , though Cr2O3 is at the extreme low end of the range [5]. Chromites (except the unusual one) have similar Fe# to the most ferroan primary chromites in ureilites [2], but distinctly lower Cr# (0.52 vs. 0.71). Metal compositions are with the range for metal in ureilites [7]. The absence of pyroxene and sulfide, and the high abundance of metal in TE 001, are unlike ureilites. One possibility is that a ferroan, chromite-bearing, pyroxene-poor ureilite was invaded (possibly due to impact) by a metallic liquid (low S content suggests very high temperature), resulting in complete melting of pyroxene and smelting of olivine, with rapid recrystallization of melted silicate as plagioclase + glass. Alternatively, a pre-existing metal-rich ureilite assemblage may have been impact melted. Additional types of data will be obtained to evaluate these hypotheses (i.e., is the metal indigenous?) and assess affinity to ureilites.

olivine↗

NASA NTRS2024

Microstructural Evolution of the Civet Cat Norite (72255)

The ‘Civet Cat Norite’ is a ~ 2.5 cm clast within the Apollo impact melt breccia sample 72255 collected during Apollo 17 EVA 2 at Boulder 1. The norite is primarily composed of plagioclase and orthopyroxene with fine-scale exsolution lamellae of augite. The plagioclase and orthopyroxene (OPX) coexist with minor quartz and augitic clinopyroxene (CPX), and accessory apatite, baddeleyite, chromite, ilmenite, loveringite, merrillite, rutile and zircon. The major minerals range from 1 to 4 mm in size and show a cataclastic texture indicated by banding of the light and dark phases]. The chemical composition of the orthopyroxene, augitic exsolution lamellae, and exsolved oxides suggest the norite crystallized in the lower crust of the Moon (10 – 70 km depth) and was subsequently excavated by impact(s). Shock pressure estimates for the norite range from 15 – 35 GPa based on maskeleynite formation within the plagioclase, kink banding in pyroxenes, and granular recrystallization in the accessory phosphates. Previous Rb-Sr and 40 Ar/ 39 Ar analyses recalculated with modern decay constants yield relatively young ages of 4.16 ± 0.05 Ga and 3.99 ± 0.03 Ga, respectively. However, recent U-Pb analyses of some zircon grains from within the Civet Cat yield an age of 4.45 ± 0.03 Ga. While this is the oldest age for any rock recovered from the Moon, the full age spread of zircon from the Civet Cat range from ca. 4.46 to 4.02 Ga, indicating variable Pb-loss and complicating interpretation of the primary age. Recent atom probe analyses indicate minimal Pb mobilization within the oldest zircon grain from Civet Cat, supporting the interpretation that these ancient zircon ages reflect the age of the norite, rather than an apparent antiquity caused by reverse discordance. To investigate the potential antiquity and deep crustal origin of the Civet Cat norite, we have undertaken high resolution microstructural analyses of the major, minor, and accessory minerals to characterize the primary igneous textures and secondary overprinting by impact and metamorphism. The employed analytical techniques include scanning electron microscope-based electron backscatter diffraction (EBSD) analyses, electron probe microanalyzer (EPMA) chemical analyses, and transmission electron microscopy (TEM) of pyroxene, plagioclase, quartz, zircon, and phosphates.

T M Erickson↗

NASA NTRS2026

Fatigue Life of Flow-Formed Aluminum 2195 and 6061 Alloys

The successful design and fabrication of metallic cryotanks for commercial aviation applications require lightweight, durable materials capable of withstanding high pressures and cryogenic temperatures through tens of thousands of thermomechanical refueling cycles. Flow forming is an advanced manufacturing technique that offers high-rate production and scalability for fabricating integrally stiffened cylinders suitable for cryotank applications. This work establishes the durability of flow-formed aluminum alloys by characterizing their fatigue life performance under conditions that mimic cryotank refueling cycles. Residual stresses in flow-formed aluminum-lithium (Al-Li) 2195-T6 cylinders were assessed using the contour method and found to be minimal. Fatigue life testing was conducted on flow-formed Al-Li 2195-T6 at room temperature and cryogenic temperatures (-321°F [-196°C]), with wrought Al-Li 2195-T6 serving as a baseline for comparison. Results showed that flow-formed materials exhibited fatigue performance comparable to or better than wrought materials, with no statistically significant differences observed between different specimen orientations relative to processing directions. Fractography revealed reduced delaminations in the flow-formed Al-Li 2195 samples as compared to wrought, indicating potential improvement to the microstructure that could result in improved service properties. Texture analysis using electron backscattered diffraction (EBSD) indicated recrystallization during heat treatment, potentially contributing to reduced delamination susceptibility. These findings demonstrating flow-formed material durability coupled with the high manufacturing efficiency of flow forming, makes flow forming an attractive process to produce aircraft cryotanks.

EBF3↗

NASA NTRS2026

Microstructural Evolution and Mechanical Properties of LP-DED NASA HR-1 – A Hydrogen Resistant AM Superalloy for Space Propulsion Applications

The National Aeronautics and Space Administration (NASA) has actively pursued metal additive manufacturing (AM) technologies for spaceflight applications since the late 2000s. AM offers transformative advantages in cost, schedule, part consolidation, and design flexibility. Among the various AM techniques, laser powder directed energy deposition (LP-DED) is particularly well suited for fabricating complex geometries with fine feature resolution. In propulsion systems that utilize high-pressure gaseous hydrogen—such as liquid hydrogen rocket engines—hydrogen environment embrittlement (HEE) presents a serious threat to material performance 1,2 . Mechanical property degradation under these conditions can compromise component reliability, especially under cyclic loading. To address this challenge, NASA developed NASA HR-1 (Hydrogen Resistant-1) as a solution for liquid rocket engine components operating in hydrogen-rich environments, using the LP-DED technique 3-9 . A key component in a liquid rocket engine is the exhaust nozzle, which is typically regeneratively cooled (regen) due to the high heat flux. NASA HR-1 was specifically developed for regen nozzle applications using hydrogen as a propellant, providing resistance to HEE, a critical issue for many materials. The AM version of NASA HR-1 was also formulated to achieve high ultimate tensile strength, along with high yield strength and ductility in this environment 5,6 . Low-cycle fatigue (LCF) is another important consideration in nozzle design, as components are expected to endure multiple starts and missions. Additionally, the LP-DED version of the alloy exhibits improved thermal conductivity compared to its wrought counterpart, which benefits nozzle cooling. Overall, NASA HR-1 offers an excellent balance of high strength, HEE resistance, LCF performance, thermal conductivity, and ductility to meet the demanding requirements of channel-cooled nozzles and other components used with hydrogen and other propellants. The LP-DED–processed NASA HR-1 requires several post-processing heat treatment steps to achieve the material properties desirable for its intended application 6 . These steps include stress relief, homogenization, solution annealing, and aging for precipitation hardening. The stress relief treatment mitigates residual stresses accumulated during the LP-DED process and minimizes the potential for distortion. Homogenization, a common step for AM materials, reduces elemental segregation and promotes recrystallization to develop a more equiaxed grain structure. The subsequent solution annealing treatment heats the part to a solid solution temperature to dissolve the undesirable η-phase that forms during cooling from homogenization, followed by rapid cooling to retain an η-phase–free microstructure. Finally, aging promotes precipitation of the strengthening γ′ phase in the alloy. The integration of compositional design and optimized thermal processing enables high-quality LP-DED NASA HR-1 components with excellent microstructural and mechanical stability. Improved chemical and microstructure homogeneity enhances ductility and fatigue resistance—both critical for safe and reliable operation in high-pressure hydrogen environments. NASA has successfully fabricated and hot-fire tested multiple subscale and full-scale channel wall nozzles using LP-DED NASA HR-1 5,6, 9-14 . These efforts included process refinements to support thin-wall construction and various channel geometries. Throughout development, several key observations emerged. After homogenization, the as-built columnar grain structure transforms into a fully equiaxed microstructure. However, subsequent treatments—such as solution annealing and aging—result in changes that are more difficult to track. The grain structure remains largely unchanged, and the γ′ precipitates, typically 5–10 nm in diameter, are beyond the resolution of scanning electron microscopy (SEM). While transmission electron microscopy (TEM) can resolve these fine precipitates, TEM sample preparation is time-consuming and difficult for LP-DED material. As an alternative, differential scanning calorimetry (DSC) offers a useful, qualitative approach to monitor precipitate evolution throughout different stages of heat treatment. The overall goal is to improve the understanding of how heat treatment affects the microstructure and mechanical performance of LP-DED NASA HR-1. This paper presents heat treatment design considerations, microstructural characterization, mechanical testing – including tensile and LCF testing in both air and hydrogen environments.

Superalloy↗

DOE OSTI2020

A FEASIBILITY STUDY ON CRACK REPAIR IN AUSTENITIC STAINLESS STEEL DRY STORAGE CANISTERS USING ISOTHERMAL FRICTION STIR WELDING

In recent time, solid state crack repair techniques in spent nuclear fuel dry storage canisters (SNF-DSC) have garnered significant interest. Plates of austenitic stainless steels are usually arc welded to fabricate the cylindrical canisters which are prone to chloride-induced stress corrosion cracking. Friction stir welding (FSW) is considered to be a potential candidate for damage repair. In this work, electrical discharge machining was used to simulate cracks in 304L stainless steel plates of 12.7 mm thickness. Subsequently, isothermal FSW was carried out at two different temperatures (725 and 825°C) in order to repair the simulated crack. Microstructure-mechanical property correlations in FSWed plates were studied in detail. Significant grain refinement observed in the stir zone (SZ) was attributed to dynamic recrystallization occurring during FSW. A comparison of Vickers microhardness showed higher hardness and homogeneity in the 725°C SZ than its 825°C counterpart. The fraction of S3 boundary is found to be low in the SZ as compared to base metal (BM). Yield strength of the joints was found to be approximately 100 MPa higher than that of the BM accompanied by a drop in ductility by a factor of 2. Residual stress profile across 825°C weld was measured using x-ray diffraction.

Bhattacharyya, Madhumanti↗