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NASA NTRS1982

Effects of cobalt on structure, microchemistry and properties of a wrought nickel-base superalloy

The effect of cobalt on the basic mechanical properties and microstructure of wrought nickel-base superalloys has been investigated experimentally by systematically replacing cobalt by nickel in Udimet 700 (17 wt% Co) commonly used in gas turbine (jet engine) applications. It is shown that the room temperature tensile yield strength and tensile strength only slightly decrease in fine-grained (disk) alloys and are basically unaffected in coarse-grained (blading) alloys as cobalt is removed. Creep and stress rupture resistances at 760 C are found to be unaffected by cobalt level in the blading alloys and decrease sharply only when the cobalt level is reduced below 8 vol% in the disk alloys. The effect of cobalt is explained in terms of gamma prime strengthening kinetics.

Jarrett, R. N.↗

NASA NTRS1991

Enstatite chondrites and achondrites as asteroidal resources

The highly reduced nature of the enstatite meteorites (chondrites and achondrites) differs from that of all other types of stony meteorites. The silicates in the enstatite meteorites contain almost no FeO. In addition, many normally lithophile elements such as Na, Ca, Mg, Cr, and Ti display chalcophilic behavior. A study of the chemistry and mineralogy of the enstatite meteorites was undertaken to determine their resource potential. On average, about 99 percent of the volume of an enstatite achondrite, or aubrite, consists of only four silicate minerals: enstatite, Na-rich plagioclase, diopside, and forsterite, with enstatite being by far the most abundant mineral. The remaining one percent of the volume consists of troilite, kamacite, and trace amounts of oldhamite, daubreelite, ferromagnesian albandite, and schreibersite. Thus, the aubrites can be considered as a possible source for large quantities of Mg, Si, and O, but are of little interest as a source of anything else. The enstatite chondrites appear to be more promising candidates for resource utilization. The chondrites are generally divided into two groups: EH (high iron, fine-grained, with abundant chondrules); and EL (low iron, coarse-grained, with little or no evidence of chondrules). Metallic Ni-Fe makes up roughly 20-25 weight percent of each type of enstatite chondrite. These meteorites are also a good source of nitrogen. This is due in part to the presence of osbornite and sinoite. The latter mineral is restricted to EL chondrites, which typically have a higher bulk nitrogen content than the EH chondrites. Three valuable metals, Cr, Mn, and Ti, are concentrated in a few distinct sulfide phases in the enstatite chondrites. These sulfide phases are troilite and niningerite in EH chondrites and troilite, daubreelite, and ferroan alabandite in EL chondrites.

Hutson, M. L.↗

NASA NTRS2002

Fine-Grained Rims in the Allan Hills 81002 and Lewis Cliff 90500 CM2 Meteorites: Their Origin and Modification

Antarctic CM meteorites Allan Hills (ALH) 8 1002 and Lewis Cliff (LEW) 90500 contain abundant fine-grained rims (FGRs) that surround a variety of coarse-grained objects. FGRs from both meteorites have similar compositions and petrographic features, independent of their enclosed objects. The FGRs are chemically homogeneous at the 10 m scale for major and minor elements and at the 25 m scale for trace elements. They display accretionary features and contain large amounts of volatiles, presumably water. They are depleted in Ca, Mn, and S but enriched in P. All FGRs show a slightly fractionated rare earth element (REE) pattern, with enrichments of Gd and Yb and depletion of Er. Gd is twice as abundant as Er. Our results indicate that those FGRs are not genetically related to their enclosed cores. They were sampled from a reservoir of homogeneously mixed dust, prior to accretion to their parent body. The rim materials subsequently experienced aqueous alteration under identical conditions. Based on their mineral, textural, and especially chemical similarities, we conclude that ALH 8 1002 and LEW 90500 likely have a similar or identical source.

Hua, X.↗

NASA NTRS2008

Transmission Electron Microscopy of Cometary Residues from Micron-Sized Craters in the Stardust Al-Foils

We report Transmission Electron Microscopy (TEM) investigations of micro-craters that originated from hypervelocity impacts of comet 81P/Wild 2 dust particles on the aluminium foil of the Stardust collector. The craters were selected by Scanning Electron Microscopy (SEM) and then prepared by Focused Ion Beam (FIB) milling techniques in order to provide electron transparent cross-sections for TEM studies. The crater residues contain both amorphous and crystalline materials in varying proportions and compositions. The amorphous component is interpreted as resulting from shock melting during the impact and the crystalline phases as relict minerals. The latter show evidence for shock metamorphism. Based on the residue morphology and the compositional variation, the impacting particles are inferred to have been dominated by mixtures of submicron olivine, pyroxene and Fe-sulfide grains, in agreement with prior results of relatively coarse-grained mineral assemblages in the aerogel collector.

Leroux, Hugues↗

NASA NTRS2009

Mineralogy of the Almahata Sitta Ureilite

Mineralogy & Petrography: Almahata Sitta, deriving from the asteroid 2008 TC3, is a coarse-grained- to porous, fine-grained, fragmental breccia with subrounded mineral fragments and olivine aggregates embedded in a cataclastic matrix of ureilitic material. Mineral fragments include polycrystalline olivine, low-calcium, pigeonite, and augite. Abundant carbonaceous aggregates containing graphite, microdiamonds and aliphatics. Kamacite, Cr-rich troilite, silica and schreibersite are abundant. The compositional range of the silicates is characteristic of the ureilites as a group, but unusually broad for an individual ureilite. The dense lithology is typical for ureilites, but the porous lithology is anomalous. In the porous lithology pore walls are largely coated by crystals of olivine. Classification: Almahata Sitta is an anomalous, polymict eucrite. Anomalous features include large compositional range of silicates, high abundance and large size of pores, crystalline pore wall linings, and fine-grained texture. Tomography reveals that the pores define thin, discontinuous "sheets" connected in three dimensions, suggesting that they outline grains that have been incompletely welded together. The crystals lining the pore walls are probably vapor phase deposits. Therefore Almahata Sitta may represent an agglomeration of coarse- to fine-grained, incompletely reduced pellets formed during impact, and subsequently welded together at high temperature.

Zolensky, Michael E.↗

DOE OSTI2020

The effect of microstructure on the relationship between grain boundary sliding and slip transmission in high purity aluminum

The relationship between grain boundary sliding (GBS) and slip transmission is investigated experimentally at grain boundaries in 99.99% aluminum with a through-thickness, coarse grained microstructure deformed in tension at 190 °C. Using scanning electron microscope enabled digital image correlation (SEM-DIC) and electron backscatter diffraction (EBSD), high resolution strain fields and microstructural information were measured to examine the influence of microstructural neighborhoods on interactions between GBS and slip transmission and strain localization. Several distinct cases are presented that highlight important microstructural factors that govern deformation near grain boundaries. The findings include (1) direct transmission and GBS were anti-compatible and facilitated by opposing boundary types (low misorientation and high energy grain boundaries respectively); (2) increased GBS activity was correlated with decreased indirect transmission behavior; (3) GBS accommodation at triple junctions was enabled by intragranular plasticity; and (4) the local intragranular plastic strain discontinuity between grains determined the magnitude of GBS gradients. Finally, this work provides insight into the nature of these mechanisms and can be used to identify strain transfer criteria that can lead to improved GBS-sensitive crystal plasticity models.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Influence of grain size on α' Cr precipitation in an isothermally aged Fe-21Cr-5Al alloy

Cr-rich α' precipitation during aging typically leads to hardening and accordingly embrittlement of FeCrAl alloys, which needs to be suppressed. The influence of grain size on α' precipitation was studied by aging coarse-grained (CG), ultra-fine grained (UFG), and nanocrystalline (NC) ferritic Kanthal-D [KD; Fe-21Cr-5Al (wt.%) alloy] at 450, 500 and 550 °C for 500 h. After aging at 450 and 500 °C, less hardening was observed in the UFG KD than in CG KD. Atom probe tomography indicated a lower number density and larger sized intragranular α' in the UFG versus the CG alloy. The smaller grain size and higher defect (vacancy and dislocation) density in the UFG KD facilitated diffusion and accordingly enhanced precipitation kinetics, leading to coarsening of precipitates, as well as saturation of precipitation at lower temperatures, as compared to those in CG KD. No hardening occurred in UFG and CG KD after aging at 550 °C, indicating that the miscibility gap is between 500 and 550 °C. NC KD exhibited softening after aging owing to grain growth. α' precipitation occurred in NC KD aged at 450 °C but not at 500 °C, indicating that miscibility gap is between 450 and 500 °C. Thus, the significantly smaller grain size in NC KD decreased the miscibility gap, as compared to that in CG and UFG KD. Finally, this is attributed to the absorption of vacancies by migrating grain boundaries during aging, suppressing α' nucleation and enhancing Cr solubility.

36 MATERIALS SCIENCE↗

DOE OSTI2023

Grain refinement in titanium prevents low temperature oxygen embrittlement

Interstitial oxygen embrittles titanium, particularly at cryogenic temperatures, which necessitates a stringent control of oxygen content in fabricating titanium and its alloys. Here, we propose a structural strategy, via grain refinement, to alleviate this problem. Compared to a coarse-grained counterpart that is extremely brittle at 77 K, the uniform elongation of an ultrafine-grained (UFG) microstructure (grain size ~ 2.0 µm) in Ti-0.3wt.%O is successfully increased by an order of magnitude, maintaining an ultrahigh yield strength inherent to the UFG microstructure. This unique strength-ductility synergy in UFG Ti-0.3wt.%O is achieved via the combined effects of diluted grain boundary segregation of oxygen that helps to improve the grain boundary cohesive energy and enhanced dislocation activities that contribute to the excellent strain hardening ability. The present strategy will not only boost the potential applications of high strength Ti-O alloys at low temperatures, but can also be applied to other alloy systems, where interstitial solution hardening results into an undesirable loss of ductility.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Dislocation density in fine grain-size spark-plasma sintered aluminum measured using high brightness synchrotron radiation

In this study, three-dimensional orientation mapping of samples of aluminum prepared by spark plasma sintering (SPS) with average grain sizes of 5 μm and 1 μm has been carried out using high-brightness synchrotron radiation, from which the geometrically necessary dislocation (GND) density has been determined. The low average measured GND density values confirm that the SPS process can be used to produce samples containing grains with dislocation density similar to that of fully recrystallized coarse-grained samples. Values of GND density are also compared to those obtained from electron back-scatter diffraction studies on the same material, highlighting the significantly higher angular resolution of the synchrotron data. For the 5 μm grain-size sample the measured GND density can account for a large fraction of the previously observed positive Hall-Petch deviation of this material. For the 1 μm grain-size sample, however, the GND-based strengthening contribution is much smaller than the reported positive Hall-Petch deviation, such that the additional strength may be reliably associated with dislocation source-limited strengthening.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Evaluation of Advanced Phased-Array Techniques: Interim Results [Slides]

Report: “Evaluation of Advanced Phased-Array Techniques: Interim Results”, August 2023 ML23216A009, PNNL-34622 Results showed that detection rate drops as microstructures/materials become more complex Standard PA had the highest detection rates overall Detection rates in the CASS-CASS mockups were lowest overall FMC had the most accurate length sizing in the fine-grained WSS mockups. All methods struggled with length sizing in coarse-grained mockups SNR vs method depended on the specimen type SNR was consistently high with standard PA SNR was consistently the lowest with PWI FMC performed best on fine-grained WSS A lack of data received from some Round Robin participants resulted in low statistics for many of the analyses.

42 ENGINEERING↗

DOE OSTI2024

Evaluation of Advanced Phased-Array Techniques: Interim Results [Slides]

42 ENGINEERING↗

NASA NTRS1988

Metal with anomalously low Ni and Ge concentrations in the Allan Hills A77081 winonaite

The Ge content of metal in the Allan Hills A77081 winonaite was determined by high-sensitivity electron microprobe analysis. By optimizing analytical conditions for Ge determination, a detection limit of about 75 ppm could be achieved. In A77081 some small kamacite grains contain less Ni and Ge and more Co than coarse-grained metal. These small grains are always associated with sulfide, raising the possibility that anomalous metal is related to eutectic melting. However, when published partition coefficients for Ni and Ge in the Fe-Ni-S system are used to model fractionation of these elements during eutectic melting, one finds that secondary metal should be enriched in Ni and depleted in Ge. Thus, the positive Ni-Ge correlation found in this study is the opposite of the expected trend. No explanation for this discrepancy has yet been found. Nonetheless, the existence of anomalous metal is an indication that A77081, and probably other winonaites as well, have undergone some fractionation. This supports the notion that the high-temperature history of winonaites is related to the formation of IAB iron meteorites, whose silicate inclusions are very similar to winonaites.

Kracher, Alfred↗

NASA NTRS2017

Ion Microprobe Measurements of Comet Dust and Implications for Models of Oxygen Isotope Heterogeneity in the Solar System

The oxygen isotopic compositions of anhydrous minerals in carbonaceous chondrites reflect mixing between a O-16-rich and O-17, O18-rich reservoir. The UV photodissociation of CO (i.e. selfshielding) has been proposed as a mass-independent mechanism for producing these isotopically distinct reservoirs. Self-shielding models predict the composition for the CO gas reservoir to be O-16-rich, and that the accreting primordial dust was in isotopic equilibrium with the gaseous reservoir [1, 2]. Self-shielding also predicts that cometary water, presumed to represent the O-17, O-18-rich reservoir, should be enriched in O-17 and O-18, with compositions of 200 -1000per mille, and that the interaction with this O-17, O-18-rich H2O reservoir altered the compositions of the primordial dust toward planetary values. The bulk composition of the solar nebula, which may be an approximation to the 16O-rich gaseous reservoir, has been constrained by the Genesis results [3]. However, material representing the O-17, O-18-rich end-member is rare [4], and dust representing the original accreting primordial dust has been challenging to conclusively identify in current collections. Anhydrous dust from comets, which accreted in the distal cold regions of the nebula at temperatures below approximately 30K, may provide the best opportunity to measure the oxygen isotope composition of primordial dust. Chondritic porous interplanetary dust particles (CP-IDPs) have been suggested as having cometary origins [5]; however, until direct comparisons with dust from a known comet parent body were made, link between CP-IDPs and comets remained circumstantial. Oxygen isotope analyses of particles from comet 81P/Wild 2 collected by NASA's Stardust mission have revealed surprising similarities to minerals in carbonaceous chondrites which have been interpreted as evidence for large scale radial migration of dust components from the inner solar nebula to the accretion regions of Jupiter- family comets [6]. These studies have been largely focused on the coarse-grained terminal particles extracted from aerogel collectors; hypervelocity capture into aerogel resulted in fine-grained material that was melted and intimately mixed with the SiO2 capture medium. Hypervelocity impacts into Al foils surrounding the aerogel tiles produced impact craters that captured material from the impactor without significant oxygen contamination, allowing for analysis of both the coarse and fine-grained components of the Wild 2 dust. To date, no particles with definitive hydrated mineralogy have been observed in Stardust samples, though this may be a result of alteration due to hypervelocity capture. High-carbon hydrated CS-IDPs have been suggested as resulting from the aqueous alteration of CP-IDPs [7], and may retain evidence for interaction with O-17, O-18-enriched "cometary" water predicted by CO self-shielding. Here we present results of oxygen isotope measurements of twelve Stardust foil craters and four C-rich hydrated IDPs [8, 9], and discuss implications for models of oxygen isotope heterogeneity in the early solar system.

Snead, C. J.↗

DOE OSTI2025

Taking three-dimensional x-ray diffraction (3DXRD) from the synchrotron to the laboratory scale

Three-dimensional x-ray diffraction (3DXRD), a rotating x-ray diffraction technique, is a powerful tool for studying the micromechanical behavior of polycrystalline materials, capable of measuring the volume, position, orientation, and strain of thousands of grains simultaneously. However, its application has been historically limited to synchrotron facilities. Here, we present the first demonstration of laboratory-scale 3DXRD (Lab-3DXRD) using a liquid-metal-jet source. Lab-3DXRD achieves accuracy comparable to synchrotron-based 3DXRD, as validated against laboratory diffraction contrast tomography (LabDCT) and synchrotron-3DXRD. Over 96% of the grains detected with Lab-3DXRD are cross-validated, particularly for coarse grains (> ~60 μm), while the results suggest that finer grains should be accessible by taking advantage of high-efficiency detectors. We further demonstrate that its sensitivity to finer grains is enhanced by incorporating pre-characterization into the analysis. This study establishes Lab-3DXRD as a practical alternative to synchrotron techniques, making 3DXRD accessible to a wider range of academic and industrial researchers.

characterization and analytical techniques↗

NASA NTRS1994

Constraints on chondrule agglomeration from fine-grained chondrule rims

Fine-grained rims around chondrules, Ca,Al-rich inclusions, and other coarse-grained components occur in most types of unequilibrated chondrites, most prominently in carbonaceous chondrites of the CM group. Based on mineralogical and petrographic investigations, it was suggested that rim structures in unequilibrated ordinary chondrites could have formed in the solar nebula by accretion of dust on the surfaces of the chondrules. Dust mantles in CM chondrites seem to have formed by accretion of dust on the surfaces of chondrules and other components during their passage through dust-rich regions in the solar nebula. Concentric mantles with compositionally different layers prove the existence of various distinct dust reservoirs in the vicinity of the accreting parent body. Despite mineralogical and chemical differences, fine-grained rims from other chondrite groups principally show striking similarities to dust mantle textures in CM chondrite. This implies that the formation of dust mantles was a cosmically significant event like the chondrule formation itself. Dust mantles seem to have formed chronologically between chondrule-producing transient heating events and the agglomeration of chondritic parent bodies. For this reason the investigation of dust mantle structures may help to answer the question of how a dusty solar nebula was transformed into a planetary system.

Metzler, K.↗

NASA NTRS1985

Mineral chemistry and origin of spinel-rich inclusions in the Allende CV3 chondrite

The present electron probe microanalysis of 20 spinel-rich inclusions in Allende indicates that the mineralogy of spinel-rich Allende inclusions is similar to that of fine grained Ca, Al-rich inclusions (CAIs) in ALH-77003 and rims on coarse grained CAIs in Allende. The mineralogy, mineral chemistry, and bulk chemistry of the inclusions indicate that they are not primitive aggregates of crystalline nebular condensates, but rather aggregates of minute concentric objects that are presently interpreted to be a fractionated distillation residue that lost Ca, Si-rich partial melt. It is suggested that interstellar dust aggregates were melted or distilled into Allende inclusions by aerodynamic drag heating, in regions of the nebula where the dust/gas ratio was so enhanced that the local oxygen fugacity was raised by several order of magnitude and liquids became thermodynamically stable.

Kornacki, A. S.↗

NASA NTRS1989

Effect of processing on fracture toughness of silicon carbide as determined by Vickers indentations

Several alpha-SiC materials were processed by hot isostatic pressing (HIPing) and by sintering an alpha-SiC powder containing boron and carbon. Several beta-SiC materials were processed by HIPing a beta-SiC powder with boron and carbon additions. The fracture toughnesses K(sub 1c) of these beta- and alpha-SiC materials were estimated from measurements of Vickers indentations. The three formulas used to estimate K(sub 1c) from the indentation fracture patterns resulted in three ranges of K(sub 1c) estimates. Furthermore, each formula measured the effects of processing differently. All three estimates indicated that fine-grained HIPed alpha-SiC has a higher K(sub 1c) than coarsed-grained sintered alpha-SiC. Hot isostatically pressed beta-SiC, which had an ultrafine grain structure, exhibited a K(sub 1c) comparable to that of HIPed alpha-SiC.

Dannels, Christine M.↗

NASA NTRS1993

Composition and maturity of the 60013/14 core

The 60013/14 double drive tube (62 cm deep) is one of three regolith cores taken 35-40 m apart in a triangular array on the Cayley plains at station 10' (LM/ALSEP), Apollo 16. This trio, which includes double drive tube 60009/10 (59 cm deep) and deep drill core 60001-7 (220 cm), is the only such array of cores returned from the Moon. The top 45 cm of 60013/14 is mature, as is surface reference soil 60601 taken nearby. Maturity generally decreases with depth, with soil below 45 cm being submature. The zone of lowest maturity (34 is less than or equal to I(sub s)/FeO is less than 50) extends from 46 to 58 cm depth, and corresponds to the distinct region of light-colored soil observed during core processing. In the other two cores, most of the compositional variation results from mixing between fine-grained, mature soil with 10-11 micro-g/g Sc and coarse-grained ferroan anorthosite consisting of greater than 99% plagioclase with less than 0.5 micro-g/g Sc. This is most evident in 60009/10 which contains a high abundance of plagioclase at about 54 cm depth (minimum Sc: 3-4 micro-g/g); a similar zone occurs in 60001-7 at 17-22 cm (MPU-C), although it is not as rich in plagioclase (minimum Sc: 6-7 micro-g/g). Compositional variations are less in 60013/14 than in the other two cores (range: 7.9-10.0 micro-g/g Sc), but are generally consistent with the 'plagioclase dilution' effect seen in 60009/10, i.e., most 60013/14 samples plot along the mixing line of 60009/10. However, a plagioclase component is not the cause of the lower maturity and lighter color of the unit at 46-58 cm depth in 60013/14. Many of the samples in this zone have distinctly lower Sm/Sc ratios than typical LM-area soils and plot off the mixing trend defined by 60009/10. This requires a component with moderately high Sc, but low-Sm/Sc, such as feldspathic fragmental breccia (FFB) or granulitic breccia. A component of Descartes regolith, such as occurs at North Ray Crater (NRC) and which is rich in FFB, could account for the composition of these soils (i.e., a 3:1 mixture of 60601 and NRC soil). It seems unlikely that NRC ejecta would occur half a meter deep at the LM station, thus this low-Sm/Sc component may result from an older, local crater that penetrated the Cayley surface layer and excavated underlying Descartes material, as did North Ray Crater. There is no evidence for such a unit or component in the other two cores. Soil below the light-colored unit (58-62) cm has 'typical' Sm/Sc ratios, but the lowest absolute Sc concentrations, i.e., it is compositionally equivalent to a mixture of surface soil and plagioclase such as that in ferroan anorthosite. This is the only soil that might be related to the plagioclase-rich units in the other two cores. Except for the mature soil at the top of each core and, perhaps, the plagioclase-rich layers, there is little compositional evidence for any common unit among the three cores. Soil corresponding to the mare-glass-bearing unit (MPU-B) and regolith-breccia-bearing unit (MPU-A) of 60001-7 do not occur in 60013/14 or 60009/10.

Korotev, Randy L.↗