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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 523 records · Page 29
All sourcesNASA NTRSDOE OSTI
NASA NTRS1994

One-step synthesis of dithiocarbamates from metal powders

Neutral metal dithiocarbamate complexes (M(NR2CS2)X) are well-known precursors to metal sulfides, a class of materials with numerous technological applications. We are involved in a research effort to prepare new precursors to metal sulfides using simple, reproducible synthetic procedures. We describe the results of our synthetic and characterization studies for M = Fe, Co, Ni, Cu. and In. For example, treatment of metallic indium with tetramethylthiuram disulfide (tmtd) in 4-methylpyridine (4-Mepy) at 25 deg C produces a new homoleptic indium (III) dithiocarbamate, In(N(CH3)2CS2)3(I), in yields of over 60 percent. The indium (III) dithiocarbamate was characterized by X-ray crystallography; (I) exists in the solid state as discrete distorted-octahedral molecules. Compound (I) crystallizes in the P1bar (No. 2) space group with lattice parameters: a = 9.282(1) A, b = 10.081(1) A, c = 12.502 A, alpha = 73.91(1) deg, beta = 70.21(1) deg, gamma = 85.8(1)deg, and Z = 2. X-ray diffraction and mass spectral data were used to characterize the products of the analogous reactions with Fe, Co, Ni, and Cu. We discuss both use of dithiocarbamates as precursors and our approach to their preparation.

Hepp, Aloysius F.↗
NASA NTRS1980

Impact-induced water loss from serpentine, nontronite and kernite

Preliminary experiments have been conducted to study shock-release of volatiles from minerals. Impact-induced loss of bound water from hydrous minerals has been observed, using infrared absorption and X-ray powder diffractometer techniques. Serpentine (Mg3Si2O5(OH)4) and nontronite (.5Ca(0.7)Fe4/(Si(7.3)Al(0.7))O20/(OH)4.nH2O) were shocked and recovered from pressures of up to 38 GPa, using one-dimensional shock reverberation techniques. Kernite (Na2B4O7.4H2O) was impacted by a spherical pyrex projectile traveling at 4.89 km/sec, which produced a peak pressure of approximately 33 GPa. The infrared absorption spectra indicate that some of the bound water from these three minerals was released as a result of shock compression and subsequent rarefaction. This evidence is supported by the recovery of small amounts of vapor from the serpentine shocked to 23.5 GPa and the nontronite shocked to 18 GPa. The recovered vapor is inferred to be water from the shocked minerals. X-ray diffraction spectra indicate no major changes in the unit cell dimensions of the two silicates, except for a decrease in the lattice constant in the c-direction of the nontronite, consistent with the loss of interlayer water.

Boslough, M. B.↗
DOE OSTI2026

Directed energy deposition of Haynes 282 nickel superalloy

Laser powder directed energy deposition was employed to fabricate Haynes® 282 Ni-based superalloy for high temperature creep testing. Material was heat treated using a single-step aging heat treatment of 800 °C for 4 h. Microstructural analysis was conducted in the as-deposited, solution-annealed, and age-hardened conditions. γ′ precipitates were absent in the as-deposited and annealed condition but formed during aging with an average size of 48.5 ± 12 nm. γ’ denuded zones ranging in thickness from 73 to 469 nm were observed adjacent to an effectively continuous grain boundary carbide film that covered 72.5% of the measured boundary length. The heat-treated material contained a high-volume fraction of TiC carbides ranging in size from 38 to 457 nm. Electron backscatter diffraction showed partial recrystallization, with 77-83% recrystallized area and a heterogeneous grain-size distribution. Creep testing at 750 °C at 300, 320, and 350 MPa revealed significantly inferior performance compared to wrought material, with higher strain rates, earlier tertiary onset, and shorter rupture lives. Fractography shows that failure was dominated by intergranular rupture. Post rupture microstructural analysis results suggest that the creep behavior was primarily governed by the non-equilibrium interface network rather than the bulk γ/γ’ matrix. In conclusion, the findings indicate that achieving wrought-like creep performance necessitates substantial improvements in the additive process, specifically focusing on enhanced homogenization, full recrystallization, and precise control over the morphology and distribution of carbides.

36 - MATERIALS SCIENCE↗
DOE OSTI2025

PROCESS-STRUCTURE-PROPERTY RELATIONSHIPS IN LASER POWDER BED FUSION PRODUCED 17-4 PH STEEL

Laser powder bed fusion (LPBF) is a metal additive manufacturing method that produces non-traditional microstructures as a result of the rapid solidification and thermal cycling inherent to the process. When using LPBF-produced material in application, these unique microstructures challenge the applicability of well developed mechanical property databases achieved by conventional heat treatments. For wider adoption of this technology, a more holistic understanding is necessary on how process attributes develop material structure, which dictate mechanical properties. This dissertation explores the process– structure–property relationships in LPBF 17-4 PH steel through systematic evaluation of atmospheric processing and heat treatment effects on microstructure and mechanical performance. Specimens were fabricated under controlled build environments, subjected to a range of solutionizing, homogenizing, and aging treatments, and characterized using optical microscopy, electron back scatter diffraction (EBSD), and X-ray diffraction (XRD) to quantify phase evolution. Tensile testing was performed to directly link heat treatment pathway and nitrogen absorption to mechanical performance. This work demonstrates where conventional heat treatment standards are applicable to LPBF 17-4 PH steel and where modifications are required. By directly correlating phase stability, nitrogen effects, and tensile response, this work provides practical guidelines for tailoring post-processing strategies. These findings underscore that successful application of LPBF 17-4 PH steel requires explicit consideration of both build environment and post-processing. By linking processing conditions to microstructure and performance, this work advances understanding of critical variables that govern reliability of additively manufactured precipitation-hardened stainless steels in demanding applications.

Brown, Benjamin [Kansas City National Security Cam↗
NASA NTRS2003

Comprehensive Study of Hydrated IDPs: X-Ray Diffraction, IR Spectroscopy and Electron Microscopic Analysis

Chondritic hydrated interplanetary dust particles (IDPs) comprise up to 50% of all IDPs collected in the stratosphere(1). Although much is known about the mineralogy, chemistry and carbon abundance of hydrated IDPs (2-4) controversies still exist regarding their formation, history, and relationship to other primitive solar system materials. Hydrated IDPs are generally believed to be derived from asteroidal sources that have undergone some degree of aqueous alteration. However, the high C contents of hydrated IDPs (by 2 to 6X CI levels (3,4) indicate that they are probably not derived from the same parent bodies sampled by the known chondritic meteorites. We report the comprehensive study of individual hydrated IDPs. The strong depletion in Ca (I) has been used as a diagnostic feature of hydrated IDPs. The particles are embedded in elemental sulfur or low viscosity epoxy and ultramicrotomed thin sections are observed using a transmission electron microscope (TEM) equipped with an energy-dispersive X-ray detector (EDX) followed by other measurements including: 1) FTIR microspectroscopy to understand the significant constraints on the organic functionality and the nature of the C-bearing phases and 2) powder X-ray difiaction using a synchrotron X-ray source to understand the bulk mineralogy of the particles.

Nakamura, K.↗
DOE OSTI2026

Boride-based Ceramic Super-high Temperature Thermocouples in Harsh Environments (Final Scientific/Technical Report)

An electromotive force (emf) can be generated along a temperature gradient between the cold end and hot end of a thermoelectric material, termed the Seebeck effect. Based on the Seebeck effect, metallic alloys have been extensively employed to detect temperatures for centuries, named thermocouples. However, commercially available thermocouple alloys suffer from limitations, such as oxidation, chemical degradation, and poor long-term stability under high-temperature harsh environments. This DOE-funded project aimed to develop high-temperature, chemically tolerant thermocouples suitable for operation in extreme environments relevant to semiconducting thermoelectric materials. The research focused on boride-based semiconducting thermoelectric compounds as candidates for next-generation thermocouples with enhanced oxidation resistance, chemical stability, and thermal robustness under conditions representative of charcoal-fired electricity facilities. During the funded years, boride materials were synthesized using an arc-plasma technique under ambient air and argon atmospheres, enabling scalable and cost-effective production compared with conventional boride fabrication methods. The synthesized borides were processed into nanostructured powders, followed by consolidation into dense bulk materials using a spark plasma sintering (SPS) bottom-up approach. Comprehensive characterization was performed, including microstructural analysis, electrical transport measurements, and optical and thermal property evaluation. Both p-type and n-type boride electric legs were fabricated and integrated into boride-based thermocouples. The thermal and irradiation stabilities of the boride nanomaterials and bulk thermoelectric materials were systematically evaluated to assess suitability for long-term operation in harsh environments. Additionally, 12 students were broadly hands-on trained spanning the full research workflow, including word processing and technical editing (e.g., LATEX for manuscript and poster preparation), data collection and analysis (using Python and related libraries and hardware interfaces), sample preparation (including arc-plasma synthesis and spark plasma sintering), and advanced characterization techniques (such as X-ray diffraction, UV–vis spectroscopy, electron microscopy, differential thermal analysis (DTA), and Seebeck coefficient measurements, etc). Overall, this project demonstrated the feasibility of boride-based thermoelectric materials as durable high-temperature thermocouples, providing a promising pathway toward robust temperature sensing technologies aligned with DOE energy infrastructure and extreme-environment monitoring needs.

20 FOSSIL-FUELED POWER PLANTS↗
DOE OSTI2024

One-Pot Coating of Ceramic Powders by Exfoliated Boron Nitride Layers with a Dense CO 2 Medium and Ultrasound-Aided Mixing

The coating or doping of substrates by two-dimensional materials to impart superior functional properties (such as improved thermal conductivity, bacterial resistance, reduced friction) is receiving increased attention. Environmentally benign, rapid and scalable coating techniques are desirable for this purpose. Here, we report a novel process for coating alumina, silicon carbide and boron carbide substrates with hexagonal boron nitride (h-BN) layers. The process consists of two sequential steps. First, h-BN layers are exfoliated from bulk h-BN in supercritical carbon dioxide (scCO 2 ) using ultrasound-aided mixing. This step is followed by self-assembly (i.e., coating) of the exfoliated h-BN on the substrates in liquid CO 2 also aided by ultrasound. The liquid CO 2 state is achieved by simply lowering the pressure and temperature of the first step below the critical point of CO 2 (P c = 72.8 atm; T c = 31.1 °C). Scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS) micrographs clearly reveal the exfoliation of h-BN under scCO 2 conditions as well as the h-BN assembly on various substrates under liquid CO 2 conditions. X-ray diffraction patterns confirm the structural integrity of the coated h-BN layers. It was also confirmed that without a transition to the liquid CO 2 phase following exfoliation in scCO 2 , there was negligible coating of h-BN on the substrates. Researchers in the field could consider this benign process to rapidly coat or dope materials with h-BN and other 2D materials to impart improved functional properties in myriad applications.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
NASA NTRS2023

Homogeneity Study of ZrC, NbC, and TaC Binary Carbide Fuels for the Application of Nuclear Thermal Propulsion

In alignment with NASA and DARPA goals, efforts towards Nuclear Thermal Propulsion (NTP) have increased in recent years. As progress is made, a main challenge still exists; the fuel in an NTP system must survive the extreme environment experienced during operating conditions. Three fuel forms have been studied including a ceramic-metallic matrix, a ceramic-ceramic matrix, and solid solution carbides. Solid solution carbides were studied previously as a fuel for NTP and was shown to be a promising technology; however, the programs were canceled before demonstration in an NTP engine test. Of the refractory metal carbides of interest, zirconium carbide (ZrC), niobium carbide (NbC) and tantalum carbide (TaC) were studied. ZrC, NbC, and TaC powders were consolidated in monocarbide (ZrC, NbC, TaC) and bi-carbide (ZrC-NbC, ZrC-TaC, NbC-TaC) forms using spark plasma sintering (SPS), with 50-50 mol% compositions of the bi-carbides of interest. The time and temperature conditions to achieve a completely homogeneous solid solution for the mixed carbides is of interest for NTP fuel applications, since this homogeneity is considered to be essential for this fuel form. Homogeneity is typically not achieved during sintering, as surface diffusion (predominant for sintering to near ideal density) tends to occur at lower temperatures than bulk volumetric diffusion (required for solute interdiffusion to achieve a homogeneous solid solution). High temperature isochronal annealing was performed to identify the conditions to achieve a chemically homogeneous sample. The solute interpenetration vs annealing temperature was quantified using energy dispersion spectroscopy (EDS) in a scanning electron microscope (SEM). X-ray diffraction (XRD) was used to accurately measure the phase stability and lattice parameter as a function of annealing conditions. The diffusion data from each sample was then used to determine self-diffusion coefficients for interdiffusion of the Nb, Zr, and Ta solutes and compared to existing literature values. The minimum annealing conditions to achieve complete chemical homogeneity for each carbide was determined.

nuclear thermal propulsion↗
DOE OSTI2024

Temperature-dependent mechanical properties and crystal plasticity parameters for additively manufactured Haynes-214 alloy: Experiments and numerical modeling

Our experimental mechanical testing data demonstrated that the additively manufactured (AM) laser powder bed fusion (L-PBF) Haynes-214 alloy exhibits non-linear mechanical properties as the temperature rises from ambient to 870 °C. Crystal plasticity (CP) simulations provide an effective approach to gaining deeper insights into microstructure-property linkages under thermomechanical loading. This method can reduce the need for costly high-temperature mechanical testing while accounting for the effects of crystallographic texture and grain morphology on the mechanical behavior of AM materials. However, calibrating a CP model is time-consuming because individual simulations are computationally expensive and hundreds (or more) of iterations over parameter sets may be required. To address this issue, we have designed a machine learning-differential evolution (ML-DE) CP framework that can accurately interpolate the tensile properties of AM L-PBF Haynes-214 alloy across a wide temperature range from ambient to 870 °C, with minimal reliance on experimental data. The framework uses electron backscatter diffraction (EBSD) measurements to generate statistically equivalent microstructural volume elements to serve as inputs to the CP modeling framework. Stress–strain curves were generated from 1000 CP simulations, which serve as the training data set for the three ML regression algorithms explored: linear, extra-trees, and multi-layer perceptron. These three regression models were independently evaluated to compare their efficiency and identify the most suitable algorithm for the given problem. Results revealed that the extra-trees ML regressor outperforms the other models in both qualitative and quantitative aspects with an R 2 of 0.98. Subsequently, the differential evolution optimization approach is employed to calibrate the ML-based CP material parameters with experimental results obtained at various temperatures. Finally, temperature-dependent CP material parameters are formulated. The effectiveness and efficiency of the designed framework are validated through comparison with experimental results, demonstrating a high degree of agreement. These calibrated parametric constitutive equations enable further use of the CP model to study the deformation behavior of this alloy under a wide range of thermo-mechanical loading conditions.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Prediction of residual stresses in additively manufactured parts using lumped capacitance and classical lamination theory

Several industries are interested in Laser Powder Bed Fusion (L-PBF) Additively Manufactured (AM) metal parts because their designs can be made arbitrarily complex while retaining bulk-type material properties. However, the residual stresses (RS) and distortions caused by the heat gradients inherent to L-PBF processes are detrimental to the structural integrity of the parts and must be taken into consideration during the part design cycle. Predicting the state of stresses in as-built 3D printed parts is a difficult problem that is typically approached with the use of transient thermomechanical Finite Element Models (FEMs). However, the nonlinearities associated with AM processes are difficult to capture in these FEMs without increasing the computational cost of the simulation, limiting their ability to be incorporated into practical design cycles. This work presents a novel analytical framework that combines lumped capacitance nonlinear heat transfer with time dependent classical lamination theory to efficiently and accurately predict RS in as-built L-PBF parts without the need of FEMs. The simulation was compared to Neutron Diffraction (ND) residual strain measurements taken at Oak Ridge National Laboratories (ORNL) as well as Synchrotron X-ray Diffraction (XRD) strain data published by the National Institute of Standards and Technology (NIST). The simulation predictions and the experimental data showed excellent agreement for the in-plane strain directions, and general agreement for the out of plane strain component, highlighting an area where further development can be implemented.

42 ENGINEERING↗
NASA NTRS2016

Calibration of the Fluorine, Chlorine and Hydrogen Content of Apatites With the ChemCam LIBS Instrument

Determining the composition of apatites is important to understand the behavior of volatiles during planetary differentiation. Apatite is an ubiquitous magmatic mineral in the SNC meteorites. It is a significant reservoir of halogens in these meteorites and has been used to estimate the halogen budget of Mars. Apatites have been identified in sandstones and pebbles at Gale crater by ChemCam, a Laser-Induced Breakdown Spectroscometer (LIBS) instrument onboard the Curiosity rover. Their presence was inferred from correlations between calcium, fluorine (using the CaF molecular band centered near 603 nm, whose detection limit is much lower that atomic or ionic lines and, in some cases, phosphorus (whose detection limit is much larger). An initial quantification of fluorine, based on fluorite (CaF2)/basalt mixtures and obtained at the LANL laboratory, indicated that the excess of F/Ca (compared to the stoichiometry of pure fluorapatites) found on Mars in some cases could be explained by the presence of fluorite. Chlorine was not detected in these targets, at least above a detection limit of 0.6 wt% estimated from. Fluorapatite was later also detected by X-ray diffraction (with CheMin) at a level of approx.1wt% in the Windjana drill sample (Kimberley area), and several points analyzed by ChemCam in this area also revealed a correlation between Ca and F. The in situ detection of F-rich, Cl-poor apatites contrasts with the Cl-rich, F-poor compositions of apatites found in basaltic shergottites and in gabbroic clasts from the martian meteorite NWA 7034, which were also found to be more Cl-rich than apatites from basalts on Earth, the Moon, or Vesta. The in situ observations could call into question one of the few possible explanations brought forward to explain the SNC results, namely that Mars may be highly depleted in fluorine. The purpose of the present study is to refine the calibration of the F, Cl, OH and P signals measured by the ChemCam LIBS instrument, initiated for F, for Cl in soils, for P, and estimate their limit of detection. For this purpose, different types of apatites and mixtures of basalt powder and apatites were analyzed using ChemCam Engineering Qualification Model (EQM) at IRAP, Toulouse. The present abstract presents the initial results from the laboratory analyses. Differences between the response function of the EQM and the Flight Model of ChemCam are still to be refined to apply these new results to the Martian dataset.

Meslin, P.-Y.↗
NASA NTRSDate not supplied

Mineralogical Trends Over the Clay-Sulfate Transition in Gale Crater from the Mars Science Laboratory CheMin Instrument

The Mars Science Laboratory Curiosity rover landed in Gale crater in 2012 to explore a sedimentary sequence in lower Aeolis Mons (informally known as Mount Sharp)that shows changes in mineralogy from orbital visible/near-infrared reflectance spectroscopy[1]. Sedimentary layers with spectral signatures of hydrated Mg sulfate overly layers with signatures of Fe/Mg smectite, a mineralogical stratigraphy that is seen in other ancient sedimentary rocks across Mars[e.g., 2-4]. Curiosity recently completed its campaign in a valley with a strong orbital signature of smectite, named Glen Torridon. Mineralogical measurements by the CheMin X-ray diffractometer(XRD), complemented by evolved gas analyses by the Sample Analysis at Mars (SAM) instrument suite, allowed the identification of abundant Fe3+-bearing dioctahedral smectite (i.e., nontronite) in Glen Torridon [5-6]. Curiosity left Glen Torridon in February 2021 and began traversing through a “clay-sulfate transition” zone on the way to the pediment and the sulfate unit[e.g., 7]. This clay-sulfate transition is defined in orbital reflectance spectroscopy as having a weak signature of hydrated Mg sulfate. Curiosity has drilled five outcrops over the traverse through the clay-sulfate transition and delivered the rock powders to CheMin for mineralogical analysis. Here, we report on the mineral assemblages of those five targets derived from CheMin XRD patterns and discuss mineralogical trends as the rover approaches the sulfate unit.

Mars↗
DOE OSTI2026

Frustration-driven magnetic correlations in the spin-$\frac{5}{2}$ triangular lattice antiferromagnet RbFe⁢(HPO 3 ) 2

Here, a detailed study of the structural and magnetic properties of a spin-5/2 triangular lattice antiferromagnet RbFe⁢(HPO 3 ) 2 is presented using x-ray diffraction, magnetization, heat capacity, and 31 P nuclear magnetic resonance (NMR) experiments on a polycrystalline sample. The crystal structure features an equilateral triangular lattice of Fe 3+ ions. The thermodynamic measurements reveal the onset of a magnetic long-range order at 𝑇 N⁢1 ≃7.8K in zero field, followed by another low-temperature field-induced ordering at 𝑇 N⁢2 in higher fields. The transition at 𝑇 N⁢1 is further confirmed from the NMR spin lattice relaxation measurements. The value of the frustration ratio (𝑓≃7) implies moderate spin frustration in the compound. The 31 P NMR spectra exhibit two distinct spectral lines corresponding to two inequivalent phosphorus sites (P1 and P2), consistent with the crystal structure. The P1 site is strongly coupled with an isotropic hyperfine coupling of 𝐴$^{iso}_{hf}$ = 0.55⁢(2)⁢ T/𝜇 B while the P2 site is weakly coupled with 𝐴$^{iso}_{hf}$ = 0.25⁢(3)⁢ T/𝜇 B with the Fe 3+ ions. The magnetic susceptibility and NMR shift data are described well assuming a spin-5/2 isotropic triangular lattice antiferromagnetic model with an average exchange coupling of 𝐽/𝑘 B = 2.8⁢(2)⁢K. Below 𝑇 N⁢1 , the spectra evolve into a nearly rectangular powder pattern, indicating a commensurate antiferromagnetic type order. The 31 P spin-lattice relaxation rate well below 𝑇N⁢1 follows a 𝑇 3 temperature dependence, implying a two-magnon Raman scattering mechanism in the ordered state. Three well-defined phase regimes are clearly ascertained in the 𝐻−𝑇 phase diagram, reflecting a weak magnetic anisotropy in the compound.

Nagpal, V. [Indian Institute of Science Education ↗
NASA NTRS2001

High-Pressure Synthesis of Metal-Ceramic Nano-Composites

The major problems in fabrication of nano-crystal line materials form nano-powders are: (1), coarsening of the initial nano-size grains, (2), insufficient densification (high concentration of pores), and, (3), conversion of diamond into graphite (for diamond-based ceramics). We have developed a novel technique of the synthesis of nano-composite materials applying very high (up to about 10 GPa) pressures. In this technique, one component is pre-compacted and placed next to another having a lower melting point temperature. The whole sample is pressed and the temperature raised above the melting point of the second component, what results in the melt getting pressed into the (nano-size) pores of the compact. Upon subsequent crystallization the melt forms the second nanophase. The process is fast, on the order of seconds, and the temperatures are relatively low what prevents, or at least significantly reduces coarsening of the starting nanophase grains. Also, conversion of diamond into graphite can be prevented. The technique allows for control of the final product properties through a proper selection of (1) the initial compact density and grain size, (2) chemical composition of the source, and (3) the temperature and pressure of the process. The application of the technique to the synthesis of SiC and diamond with Si, Ge, and different metals. Results of the in-situ investigation of the synthesis process by synchrotron X-ray diffraction technique will be presented.

Gierlotka, S.↗
NASA NTRS1993

Reaction of YBa2Cu3O(7-beta) with Gold, Silver, Bismuth and Lead: Substitution Chemistry and Composite Fabrication

The reaction of YBa2Cu3O(7-beta) with Au, Ag, Bi, and Ph ions or metal is described. Three types of materials were produced: a well-defined series of homogeneous superconductors was obtained for Au ion substitution with little effect on T(sub c); attempted Ag and Bi ion substitution resulted in multi-phase samples with slightly enhanced T(sub c); finally, attempts to produce superconducting metal/superconducting ceramic composites with Pb and Bi powders resulted in multi-phase samples with drastically diminished superconducting properties. For Au- substituted superconductors, YBa2(Cu(l-x)Au(x))3O(7-beta), a substitution series (x = 0 - 0.1) has been synthesized. For x = 0.1 there was no change in the a and b lattice parameters (a = 3.826 A and b = 3.889 A) but a 0.06 A c axis expansion to 11.75 A was observed. The valence of Cu and Au in YBa2Au(0.3)Cu(2.7)O(7-beta) was investigated using X-ray Absorption Near-Edge Structure (XANES). X-ray studies indicate that Au goes into the Cu(l) site and Cu K edge XANES shows that this has little effect on the oxidation state of the remaining copper. A small effect on T(sub c) is observed (T(sub c) = 89 K for x = 0.10). Ag and Bi addition results in a rise in T(sub c) and a decrease in (delta)T(sub c) at low levels (x = 0.10 Ag, T(sub c) = 94 K and (delta)T(sub c) = 0.5 K; x = 0.02 Bi, T(sub c) = 94 K and (delta)T(sub c) = 1K) relative to typical values for YBa2Cu3O(7-beta) (T(sub c) = 91 K, (delta)T(sub c) = 2 K). Attempts at fabrication of Pb- and Pb(1-x)Bi(x)-superconductor composites are described. Cold pressing followed by low temperature (200 C) sintering resulted in a composite which excluded flux below 90 K but did not show zero electrical resistance until the metal (alloy) superconducting transition. X-ray diffraction showed the presence of pervoskite and metal. Processing at moderate (450 C) or high (950 C) temperatures resulted in oxygen-depleted pervoskite and/or metal oxides. These materials displayed greatly degraded superconducting properties. Processing at 800 C resulted in high T(sub c) only for composites containing greater than 90% weight fraction ceramic. Reaction of metal with YBa2Cu3O(7-beta) formed superconducting lead/bismuth-based oxides and other binary oxides.

Hepp, Aloysius F.↗
NASA NTRS2015

Diagenetic Mineralogy at Gale Crater, Mars

Three years into exploration of sediments in Gale crater on Mars, the Mars Science Laboratory rover Curiosity has provided data on several modes and episodes of diagenetic mineral formation. Curiosity determines mineralogy principally by X-ray diffraction (XRD), but with supporting data from thermal-release profiles of volatiles, bulk chemistry, passive spectroscopy, and laser-induced breakdown spectra of targeted spots. Mudstones at Yellowknife Bay, within the landing ellipse, contain approximately 20% phyllosilicate that we interpret as authigenic smectite formed by basalt weathering in relatively dilute water, with associated formation of authigenic magnetite as in experiments by Tosca and Hurowitz [Goldschmidt 2014]. Varied interlayer spacing of the smectite, collapsed at approximately 10 A or expanded at approximately 13.2 A, is evidence of localized diagenesis that may include partial intercalation of metal-hydroxyl groups in the approximately 13.2 A material. Subsequent sampling of stratigraphically higher Windjana sandstone revealed sediment with multiple sources, possible concentration of detrital magnetite, and minimal abundance of diagenetic minerals. Most recent sampling has been of lower strata at Mount Sharp, where diagenesis is widespread and varied. Here XRD shows that hematite first becomes abundant and products of diagenesis include jarosite and cristobalite. In addition, bulk chemistry identifies Mg-sulfate concretions that may be amorphous or crystalline. Throughout Curiosity's traverse, later diagenetic fractures (and rarer nodules) of mm to dm scale are common and surprisingly constant and simple in Ca-sulfate composition. Other sulfates (Mg,Fe) appear to be absent in this later diagenetic cycle, and circumneutral solutions are indicated. Equally surprising is the rarity of gypsum and common occurrence of bassanite and anhydrite. Bassanite, rare on Earth, plays a major role at this location on Mars. Dehydration of gypsum to bassanite in the dry atmosphere of Mars has been proposed but considered unlikely based on lab studies of dehydration kinetics in powdered samples. Dehydration is even less likely for bulk vein samples, as lab data show dehydration rates one to two orders of magnitude slower in bulk samples than in powders. On Mars, exposure ages of 100 Ma or more may be a significant factor in dehydration of hydrous phases.

Vaniman, David↗
NASA NTRS2004

Investigation of the Environmental Durability of a Powder Metallurgy Material

PM304 is a NASA-developed composite powder metallurgy material that is being developed for high temperature applications such as bushings in high temperature industrial furnace conveyor systems. My goal this summer was to analyze and evaluate the effects that heat exposure had on the PM304 material at 500 C and 650 C. The material is composed of Ni-Cr, Ag, Cr2O3, and eutectic BaF2-CaF2. PM304 is designed to eliminate the need for oil based lubricants in high temperature applications, while reducing friction and wear. However, further investigation was needed to thoroughly examine the properties of PM304. The effects of heat exposure on PM304 bushings were investigated. This investigation was necessary due to the high temperatures that the material would be exposed to in a typical application. Each bushing was cut into eight sections. The specimens were heated to 500 C or 650 C for time intervals from 1 hr to 5,000 hrs. Control specimens were kept at room temperature. Weight and thickness measurements were taken before and after the bushing sections were exposed to heat. Then the heat treated specimens were mounted and polished side by side with the control specimens. This enabled optical examination of the material's microstructure using a metallograph. The specimens were also examined with a scanning electron microscope (SEM). The microstructures were compared to observe the effects of the heat exposure. Chemical analysis was done to investigate the interactions between Ni-Cr and BaF2-CaF2 and between Cr2O3 and BaF2-CaF2 at high temperature. To observe this, the two compounds that were being analyzed were mixed in a crucible in varied weight percentages and heated to 1100 C in a furnace for approximately two hours. Then the product was allowed to cool and was then analyzed by X-ray diffraction. Interpretation of the results is in progress.

Ward, LaNita D.↗
NASA NTRS2018

Plasticity and Damage Modeling of Stress Asymmetry and Dynamic Behavior of AFS Additive Manufactured Aluminum Alloy 2219

The Solid State Additive Manufacturing (AM) process referred as MELD that fabricated the samples in this study, provides a new path for repairing, coating, joining and additive manufacturing metals and metal matrix composites. This research will be the first application of a physics-based microstructure dependent internal state variable (ISV) plasticity and damage material model to capture the mechanical response of an AM Aluminum Alloy (AA) 2219 via the MELD process. In this research, a microstructure-based internal state variable (ISV) plasticity-damage model was used to capture the mechanical behavior of AFS 2219 aluminum alloy. Aeroprobe Corporation, creator and patent holder for the MELD process, fabricated the material by pushing a solid filler rod of AA2219-T861 material through a hollow rotating tool onto an AA2219 T851 plate substrate. As feedstock, solid or powder precursor metals are pushed through a nonconsumable rotating cylindrical tool. Herein, added layers are deposited and metallurgically bonded to substrate material or previously deposited layers by the heat generated from the rotating tool through plastic deformation of the filler material. Once a layer has been added, the tool height increases, and starts the deposition of the next layer. This process results in beneficial properties such as grain refinement, homogenization and reduced porosity (fully dense). This process will experience temperatures similar to those in the weld nugget zone (WNZ) in friction stir welding (FSW), ranging from 0.6-0.9 Tm, with Tm being the melting point of the material. MELD is highly scalable with AA deposition rates reaching over 1000 cm3/hr, which allows for MELD being used for repairs, coatings, and building components. A motivating factor driving the research for physics-based history dependent material modeling of MELD components is the ability to accurately capture the stress-state and strain rate dependence in the material caused by variations in material microstructure from the MELD processing of new or repaired components. The ISV model incorporates microstructural content and is consistent with continuum level kinematics, kinetics, and thermodynamics. These features allow the ISV model to capture large deformations at the structural scale using the kinematic and isotropic hardening, while microscale damage is obtained from the microstructural features. The benefits of the ISV model arise from the inclusion of structure-property relationships identified from microstructural characterization and experimentation. The Bauschinger effect (BE) is an important concept, vital in the accurate prediction of cyclic stress-strain response of ductile materials such as metals. The ISV model has been successfully used to capture the behavior and damage, and the BE of different aluminum alloys and steels. The ISV model uses kinematic and isotropic hardening to help capture deformations of the material at the macro scale. To understand this hardening relationship, calculating the kinematic and isotropic hardening relationship in the material is warranted for a high-fidelity model. Electron Backscattered Diffraction (EBSD) was used to characterize the as-fabricated microstructure, where a fully-dense equiaxed grain morphology with average grain size of 2.5 μm was observed. Microhardness mapping of the as-built structures, monotonic tension and compression experiments at both quasi-static (0.001/s) strain rates, tension-followed-by-compression and compression-followed-by-tension experiments were performed to obtain the set of plasticity and damage constants necessary to capture strain rate and stress state behavior of this additive material. To calibrate the plasticity-damage model, a single set of constants were determined to capture the different stress states the MELD AA2219. One set of the constants was determined from experimental true stress-strain curves for the tension and compression data. Additionally, microstructural information and data from the open literature were used as the other model constants. This research is a first of its kind for AFS AA2219, includes correlating the ISV model to the monotonic experimental results that capture the isotropic and kinematic plasticity mechanical response.

Rivera, O. G.↗