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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 973 records · Page 54
All sourcesNASA NTRSDOE OSTI
DOE OSTI2024

Post-irradiation examination of commercial tantalum alloys following neutron irradiation

Post irradiation examination of two commercial tantalum alloys (based on Ta-8 %W) revealed significant irradiation hardening following neutron irradiation in the High Flux Isotope Reactor at Oak Ridge National Laboratory. Tensile samples of commercial Ta alloys T-111 and ASTAR-811C were irradiated to a total neutron fluence (E > 0.1 MeV) in the range (2–4)x10 21 n/cm 2 (0.39–0.75 dpa) at an irradiation temperature near 900 °C. Tensile testing conducted at room temperature and at 800 °C revealed significant irradiation hardening under all test conditions. Samples that were tensile tested at room temperature exhibited brittle failure, whereas ductility was maintained for elevated temperature testing. The irradiation hardening and embrittlement noted for both alloys was attributed to irradiation-induced dislocation loop formation as confirmed through scanning transmission electron microscopy analysis. Corresponding energy dispersive x-ray spectroscopy revealed radiation-induced segregation of Hf in these loop populations. This Hf enrichment is shown to result in eventual co-precipitation of elongated (Hf,O)-rich precipitates along the dislocation loops. Further, these results show that irradiation hardening is enhanced via irradiation-enhanced precipitation at elevated irradiation temperatures. Consequently, the minimum recommended operating temperature window for Ta alloys should be increased to account for observed hardening/embrittlement at irradiation temperatures as high as 900 °C (1,173 K).

36 MATERIALS SCIENCE↗
DOE OSTI2014

NanoSIMS, TEM, and XANES studies of a unique presolar supernova graphite grain

We report on isotopic and microstructural investigations of a unique presolar supernova (SN) graphite grain, referred to as G6, isolated from the Orgueil CI chondrite. G6 contains complex heterogeneities in its isotopic composition and in its microstructure. Nano-scale secondary ion mass spectrometer isotope images of ultramicrotome sections reveal heterogeneities in its C, N, and O isotopic compositions, including anomalous shell-like structures. Transmission electron microscope studies reveal a nanocrystalline core surrounded by a turbostratic graphite mantle, the first reported nanocrystalline core from a low-density SN graphite grain. Electron diffraction analysis shows that the nanocrystalline core consists of randomly oriented 2-4 nm graphene particles, similar to those in cores of high-density (HD) presolar graphite grains from asymptotic giant branch stars. G6's core also exhibits evidence for planar stacking of these graphene nano-sheets with a domain size up to 4.5 nm, which was unobserved in the nanocrystalline cores of HD graphite grains. We also report on X-ray absorption near-edge structure measurements of G6. The complex isotopic- and micro-structure of G6 provides evidence for mixing and/or granular transport in SN ejecta.

79 ASTRONOMY AND ASTROPHYSICS↗
DOE OSTI2011

Menzerite-(Y) a New Species {(Y REE)(Ca Fe2plus)2}[(Mg Fe2plus)(Fe3plus Al)](Si3)O12 from a Felsic Granulite Parry Sound Ontario and a New Garnet End-member (Y2Ca)Mg2(SiO4)3

Menzerite-(Y), a new mineral species, forms reddish brown cores, n = 1.844 (20), up to 70 {micro}m across, rimmed successively by euhedral almandine containing up to 2.7 wt% Y{sub 2}O{sub 3} and by K-feldspar in a felsic granulite on Bonnet Island in the interior Parry Sound domain, Grenville Orogenic Province, Canada. It is named after Georg Menzer (1897-1989), the German crystallographer who solved the crystal structure of garnet. Single-crystal X-ray-diffraction results yielded space group Ia3d, a = 11.9947(6) {angstrom}. An electron-microprobe analysis of the grain richest in Y (16.93 wt% Y{sub 2}O{sub 3}) gave the following formula, normalized to eight cations and 12 oxygen atoms: {l_brace}Y{sub 0.83}Gd{sub 0.01}Dy{sub 0.05}Ho{sub 0.02}Er{sub 0.07}Tm{sub 0.01}Yb{sub 0.06}Lu{sub 0.02}Ca{sub 1.37}Fe{sub 0.49}{sup 2+}Mn{sub 0.07}{r_brace} [Mg{sub 0.55}Fe{sub 0.42}{sup 2+}Fe{sub 0.58}{sup 3+}Al{sub 0.35} V{sub 0.01}Sc{sub 0.01}Ti{sub 0.08}](Si{sub 2.82}Al{sub 0.18})O{sub 12}, or {l_brace}(Y,REE)(Ca,Fe{sup 2+}){sub 2}{r_brace}[(Mg,Fe{sup 2+})(Fe{sup 3+},Al)](Si{sub 3})O{sub 12}. Synchrotron micro-XANES data gave Fe{sup 3+}/{Sigma}Fe = 0.56(10) versus 0.39(2) calculated from stoichiometry. The scattering power refined at the octahedral Y site, 17.68 epfu, indicates that a relatively light element contributes to its occupancy. Magnesium, as determined by electron-microprobe analyses, would be a proper candidate. In addition, considering the complex occupancy of this site, the average Y-O bond length of 2.0244(16) {angstrom} is in accord with a partial occupancy by Mg. The dominance of divalent cations with Mg > Fe{sup 2+} and the absence of Si at the octahedral Y site (in square brackets) are the primary criteria for distinguishing menzerite-(Y) from other silicate garnet species; the menzerite-(Y) end-member is {l_brace}Y{sub 2}Ca{r_brace}[Mg{sub 2}](Si{sub 3})O{sub 12}. The contacts of menzerite-(Y) with almandine are generally sharp and, in places, cuspate. It is interpreted to have equilibrated with ferrosilite, augite, quartz, oligoclase, allanite-(Ce), magnetite, ilmenite and fluorapatite, in the absence of almandine, on the prograde path at 7-8.5 kbar and T {approx} 700-800 C, and subsequently dissolved incongruently in an anatectic melt to form almandine, most likely, at P {approx} 8.5-9.5 kbar and T {approx} 800-850 C.

58 GEOSCIENCES↗
DOE OSTI2014

Investigation of the GaN-on-GaAs interface for vertical power device applications

GaN layers were grown onto (111) GaAs by molecular beam epitaxy. Minimal band offset between the conduction bands for GaN and GaAs materials has been suggested in the literature raising the possibility of using GaN-on-GaAs for vertical power device applications. I-V and C-V measurements of the GaN/GaAs heterostructures however yielded a rectifying junction, even when both sides of the junction were heavily doped with an n-type dopant. Transmission electron microscopy analysis further confirmed the challenge in creating a GaN/GaAs Ohmic interface by showing a large density of dislocations in the GaN layer and suggesting roughening of the GaN/GaAs interface due to etching of the GaAs by the nitrogen plasma, diffusion of nitrogen or melting of Ga into the GaAs substrate.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2023

The Crucial Role of Sb 2 F 10 in the Chemical Synthesis of F 2

The purely chemical synthesis of fluorine is a spectacular reaction which for more than a century had been believed to be impossible. In 1986, it was finally experimentally achieved, but since then this important reaction has not been further studied and its detailed mechanism had been a mystery. The known thermal stability of MnF 4 casts serious doubts on the originally proposed hypothesis that MnF 4 is thermodynamically unstable and decomposes spontaneously to a lower manganese fluoride and F 2 . This apparent discrepancy has now been resolved experimentally and by electronic structure calculations. It is shown that the reductive elimination of F 2 requires a large excess of SbF 5 and occurs in the last reaction step when in the intermediate [SbF 6 ][MnF 2 ][Sb 2 F 11 ] the addition of one more SbF 5 molecule to the [SbF 6 ] - anion generates a second tridentate [Sb 2 F 11 ] - anion. The two tridentate [Sb 2 F 11 ] - anions then provide six fluorine bridges to the Mn atom thereby facilitating the reductive elimination of the two fluorine ligands as F 2 .

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2013

Nanostructural and electronic properties of polytypes in InN nanocolumns

Transmission electron microscopy techniques and density functional theory calculations were employed to investigate the nanostructural and electronic properties of InN polytypes observed in InN nanocolumns, grown on Si(111) by molecular beam epitaxy. Moiré fringes and alternating hexagonal and cubic lattice stacking sequences along the c-axis, observed among the wurtzite layers, implied the presence of different structures embedded in the basic 2H structure of the nanocolumns. Quantitative electron diffraction analysis and high-resolution image simulations verified the coexistence of the wurtzite structure with the 4H, 6H, and the 3C zinc-blende structural polytypes. Total energies calculations established the 2H wurtzite structure as the most stable polytype. The band gap of all polytypes was found direct with the energies and the band gaps of the 4H (E{sub g} = 0.64 eV) and 6H (E{sub g} = 0.60 eV) structures calculated between the corresponding values of the 2H (E{sub g} = 0.75 eV) and 3C (E{sub g} = 0.49 eV) basic structures. Theoretical and experimental analysis showed that at the initial stages of growth InN nanocolumns were under tensile strain along both the basal plane and growth direction. Structural polytypes were then introduced in the form of embedded inclusions to accommodate the excess tensile strain along the growth direction, allowing the entire process of polymorphism to be the dominant strain relaxation mechanism of InN nanocolumns. Moreover, the lattice and energetic properties and band gap values of InN polytypes showed a linear dependence on hexagonality, while the presence of polytypes led to a characteristic broadening of the photoluminescence emission peak toward lower emission energies.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Microstructural Characterization of FeCrAl C26M Tubes

The present report summarizes the initial nanoindentation characterization of a FeCrAl alloy, C26M. Microstructural analysis using electron backscatter diffraction showed a highly textured system with the axial surface favoring orientations near the [110] and the longitudinal surface near the [111]. A large spread of grain sizes was observed from a few μm’s to 100 μm with an average grain size of ~70 μm. Nanoindentation with a Berkovich tip measured a similar hardness and modulus of ~4.4 GPa and ~240 GPa on the two surfaces, respectively. Mounting specimens in epoxy was found to be the cause of a lower stiffness and, consequently, a lower hardness and modulus value. Spherical nanoindentation was measured on the longitudinal surface of the tube to determine the nanoindentation modulus and nanoindentation yield strength. Using a 10 μm tip, the measured modulus was ~220 GPa and the yield strength was ~1.4 GPa. Indentation with a 100 μm tip resulted in a measured modulus value of ~220 GPa and yield strength of ~1.1 GPa. Some early characterization of the differences in spherical nanoindentation response of the axial and longitudinal surfaces showed a small difference between the two, but a more detailed analysis with a stiffer mounting configuration is needed to draw conclusions.

36 MATERIALS SCIENCE↗
NASA NTRS1988

On the need for space tests of plasma contactors as electron collectors

An analysis is presented of laboratory experiments that have shown that hollow plasma sources can provide low-impedance contact with a background plasma. In particular, some experiments show an report an 'ignited mode' of electron collection using plasma sources where almost an ampere was collected at a potential of 100 volts. The experimental results are compared with theoretical and computational models of plasma layers. Preliminary results indicate that the measured potential profiles and collected currents during the 'ignited mode' correspond to an increase in the background plasma thermal current of more than an order of magnitude. The results imply that the 'ignited mode' results are substantially impacted by the laboratory electron source and the tank size. Only experiments performed in space will be able to provide the correct boundary conditions for reliably testing high electron collection by plasma contactors.

Katz, Ira↗
DOE OSTI2016

Exploring Electron/Proton Transfer and Conformational Changes in the Nitrogenase MoFe Protein and FeMo-cofactor Through Cryoreduction/EPR Measurements

Here, we combine cryoreduction/annealing/EPR measurements of nitrogenase MoFe protein with results of earlier investigations to provide a detailed view of the electron/proton transfer events and conformational changes that occur during early stages of [e - /H + ] accumulation by the MoFe protein. This includes reduction of (i) the non-catalytic state of the iron-molybdenum cofactor (FeMo-co) active site that is generated by chemical oxidation of the resting-state cofactor (S = 3/2)) within resting MoFe (E 0 ), and (ii) the catalytic state that has accumulated n =1 [e - /H + ] above the resting-state level, denoted E 1 (1H) (S ≥ 1) in the Lowe-Thorneley kinetic scheme. FeMo-co does not undergo a major change of conformation during reduction of oxidized FeMo-co. In contrast, FeMo-co undergoes substantial conformational changes during the reduction of E 0 to E 1 (1H), and of E 1 (1H) to E 2 (2H) (n = 2; S = 3/2). The experimental results further suggest that the E 1 (1H) → E 2 (2H) step involves coupled delivery of a proton and electron (PCET) to FeMo-co of E 1 (H) to generate a non-equilibrium S = ½ form E 2 (2H)*. This subsequently undergoes conformational relaxation and attendant change in FeMo-co spin state, to generate the equilibrium E 2 (2H) (S = 3/2) state. Unexpectedly, these experiments also reveal conformational coupling between FeMo-co and P-cluster, and between Fe protein binding and FeMo-co, which might play a role in gated ET from reduced Fe protein to FeMo-co.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2014

Improved gas sensing and dielectric properties of Fe doped hydroxyapatite thick films: Effect of molar concentrations

Highlights: • We report improved gas sensing and dielectric characteristics of Fe ion exchanged HAp films. • Fe doped HAp film shows maximum gas response at relatively lower temperature. • Response and gas uptake capacity of sensors is improved for appropriate amount of Fe ions in HAp matrix. • Fe-HAp films exhibit remarkable improvement in dielectric properties compared to pure HAp. • Fe doped HAp films show significant improvement in gas sensing as well as in dielectric properties. - Abstract: In the present work Fe doped hydroxyapatite (Fe-HAp) thick films has been successfully utilized to improve the gas sensing as well as its dielectric properties. Initially, HAp nano powder is synthesized by chemical precipitation process and later on Fe ions are doped in HAp by ion exchange process. Structural and morphological modifications are observed by means of X-ray diffraction and scanning electron microscopy analysis. The sensing parameters such as operating temperature, response/recovery time and gas uptake capacity are experimentally determined. The Fe-HAp (0.05 M) film shows improved CO and CO{sub 2} gas sensing capacity at lower operating temperature compared to pure HAp. Moreover, variation of dielectric constant and dielectric loss for pure and Fe-HAp thick films are studied as a function of frequency in the range of 10 Hz–1 MHz. The study reveals that Fe doped HAp thick films improve the sensing and dielectric characteristics as compared to pure HAp.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Effect of sputtering pressure on microstructure and bolometric properties of Nb:TiO{sub 2−x} films for infrared image sensor applications

This study aims to investigate the influence of the sputtering pressure (P{sub S}) on Nb:TiO{sub 2−x} films to enhance the bolometric properties. A decrease in the growth rate with the sputtering pressure was perceived in amorphous Nb:TiO{sub 2−x} films. The incorporation of oxygen with P{sub S} was confirmed in an X-ray photo electron spectroscopy analysis. The electrical resistivity was increased with an increase in P{sub S} due to a decrease in the number of oxygen vacancies. The linear I-V characteristics confirmed the ohmic contact behavior between the Nb:TiO{sub 2−x} layer and the electrode material. The present investigation finds that the sample with lower resistivity has good bolometric properties with low noise and high universal bolometric parameters. Finally, the Nb:TiO{sub 2−x} sample deposited at a sputtering pressure of 2 mTorr shows better bolometric properties than other materials for infrared image sensor applications.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2011

Dispersion Morphology of Poly(methyl acrylate)/Silica Nanocomposites

Nearly monodisperse poly(methyl acrylate) (PMA) and spherical SiO{sub 2} nanoparticles (NP, d = 14 {+-} 4 nm) were co-cast from 2-butanone, a mutually good solvent and a displacer of adsorbed PMA from silica. The effects of NP content and post-casting sample history on the dispersion morphology were found by small-angle X-ray scattering supplemented by transmission electron microscopy. Analysis of the X-ray results show that cast and thermally annealed samples exhibited a nearly random particle dispersion. That the same samples, prior to annealing, were not well-dispersed is indicative of thermodynamic miscibility during thermal annealing over the range of NP loadings studied. A simple mean-field thermodynamic model suggests that miscibility results primarily from favorable polymer segment/NP surface interactions. The model also indicates, and experiments confirm, that subsequent exposure of the composites to the likely displacer ethyl acetate results in entropic destabilization and demixing into NP-rich and NP-lean phases.

36 MATERIALS SCIENCE↗
DOE OSTI2012

High-Performance LiNi0.5Mn1.5O4 Spinel Controlled by Mn3+ Concentration and Site Disorder

The influences of Mn3+ ions on the properties of high voltage spinel LiNi0.5Mn1.5O4 is systematically investigated in this work. The content of Mn3+ ions in the spinel is tuned by further annealing of the sample or partially substitution of Ni2+ in the lattice structure. The former decreases the amount of Mn3+ while the latter increases Mn3+ concentration, which has been confirmed by both X-ray diffraction (XRD) and electron diffraction analysis. It has also been experimentally and theoretically proven that Mn3+ ions are directly related to the disordering between Ni2+ and Mn4+ on the octahedral sites in the spinel structure which facilitates the transportation of Li+ ions especially at elevated current densities. An extremely cycling stability as well as good rate capability have been observed in the Cr-substituted spinel confirming that an appropriate amount of Mn3+ ions is the key for a high performance high voltage spinel.

36 MATERIALS SCIENCE↗
DOE OSTI2011

Innate immune system still works at diapause, a physiological state of dormancy in insects

Highlights: {yields} Two major types of cells are present in the body fluid isolated from the thoracic region of a diapausing pupa. {yields} Phagocytosis and encapsulation by these cells were observed when latex beads as foreign targets were microinjected into a pupa. {yields} Such behavior by these cells was still observed even when pupae were continuously chilled at 4 {sup o}C. {yields} Innate cellular reactions can work in diapausing insects in a dormant state. -- Abstract: Diapause is most often observed in insects and is a physiologically dormant state different from other types of dormancy, such as hibernation. It allows insects to survive in harsh environments or extend longevity. In general, larval, pupal, or adult non-diapausing insects possess an innate immune system preventing the invasion of microorganisms into their bodies; however, it is unclear whether this system works under the dormant condition of diapause. We here report the occurrence of innate cellular reactions during diapause using pupae of a giant silkmoth, Samia cynthia pryeri. Scanning electron microscopic analysis demonstrated the presence of two major types of cells in the body fluid isolated from the thoracic region of a pupa. Phagocytosis and encapsulation, characteristics of innate cellular reactions, by these cells were observed when latex beads as foreign targets were microinjected into the internal portion of a pupa. Such behavior by these cells was still observed even when pupae were continuously chilled at 4 {sup o}C. Our results indicate that innate cellular reactions can work in diapausing insects in a dormant state.

60 APPLIED LIFE SCIENCES↗
DOE OSTI2016

Big Data Analytics for Scanning Transmission Electron Microscopy Ptychography

Electron microscopy is undergoing a transition; from the model of producing only a few micrographs, through the current state where many images and spectra can be digitally recorded, to a new mode where very large volumes of data (movies, ptychographic and multi-dimensional series) can be rapidly obtained. In this paper, we discuss the application of so-called “big-data” methods to high dimensional microscopy data, using unsupervised multivariate statistical techniques, in order to explore salient image features in a specific example of BiFeO 3 domains. Remarkably, k-means clustering reveals domain differentiation despite the fact that the algorithm is purely statistical in nature and does not require any prior information regarding the material, any coexisting phases, or any differentiating structures. While this is a somewhat trivial case, this example signifies the extraction of useful physical and structural information without any prior bias regarding the sample or the instrumental modality. Further interpretation of these types of results may still require human intervention. Finally, however, the open nature of this algorithm and its wide availability, enable broad collaborations and exploratory work necessary to enable efficient data analysis in electron microscopy.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Disruption of crystalline structure of Sn3.5Ag induced by electric current

This study presented the disruption of the Sn and Ag{sub 3}Sn lattice structures of Sn3.5Ag solder induced by electric current at 5–7 × 10{sup 3} A/cm{sup 2} with a high resolution transmission electron microscope investigation and electron diffraction analysis. The electric current stressing induced a high degree of strain on the alloy, as estimated from the X-ray diffraction (XRD) peak shift of the current stressed specimen. The XRD peak intensity of the Sn matrix and the Ag{sub 3}Sn intermetallic compound diminished to nearly undetectable after 2 h of current stressing. The electric current stressing gave rise to a high dislocation density of up to 10{sup 17}/m{sup 2}. The grain morphology of the Sn matrix became invisible after prolonged current stressing as a result of the coalescence of dislocations.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2014

Laser assisted high entropy alloy coating on aluminum: Microstructural evolution

High entropy alloy (Al-Fe-Co-Cr-Ni) coatings were synthesized using laser surface engineering on aluminum substrate. Electron diffraction analysis confirmed the formation of solid solution of body centered cubic high entropy alloy phase along with phases with long range periodic structures within the coating. Evolution of such type of microstructure was a result of kinetics associated with laser process, which generates higher temperatures and rapid cooling resulting in retention of high entropy alloy phase followed by reheating and/or annealing in subsequent passes of the laser track giving rise to partial decomposition. The partial decomposition resulted in formation of precipitates having layered morphology with a mixture of high entropy alloy rich phases, compounds, and long range ordered phases.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2018

Characteristics of Calcium-Aluminate Slags and Pig Iron Produced from Smelting-Reduction of Low-Grade Bauxites

Low-grade bauxite ores are not favorable in the conventional Bayer process for alumina production, as they are producing more bauxite residue (red mud) and accompanying lower alumina yield than high-grade ores. In the current study, the thermodynamics and characterization of calcium-aluminate slags and pig iron produced from smelting reduction of high iron- and silica-containing bauxites are studied. Coke and limestone are used to reduce the iron oxide and adjust the basicity of slag during smelting. There is evidence that complete iron separation from bauxite is feasible through smelting-reduction process, and up to 99.9 pct of iron can be eliminated. Moreover, it is shown that the partial separation of silicon, titanium, and other elements from the Al{sub 2}O{sub 3}-containing slag occurs. The phase compositions and the distribution of elements between the metal and slag phases provide information about the high-temperature behavior of the bauxite components during smelting reduction. Employing electron microscopy analysis, it is indicated that the morphologies of CaO·Al{sub 2}O{sub 3}, 12CaO·7Al{sub 2}O{sub 3}, 2CaO·Al{sub 2}O{sub 3}·SiO{sub 2}, and CaO·Al{sub 2}O{sub 3}·SiO{sub 2} phases in the slag, as well as the complex oxides of Ca-Al-Si-Ti in the slag behave differently as the mass ratio of Al{sub 2}O{sub 3}/(Fe{sub 2}O{sub 3 }+ SiO{sub 2}) in the bauxite changes. It is also shown that the phases of slag produced from smelting-reduction below 5 K s{sup −1} of cooling rate are proper for further leaching process.

36 MATERIALS SCIENCE↗