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At least 775 records · Page 43

NiAl alloys for structural uses

Alloys based on the intermetallic compound NiAl are of technological interest as high temperature structural alloys. These alloys possess a relatively low density, high melting temperature, good thermal conductivity, and (usually) good oxidation resistance. However, NiAl and NiAl-base alloys suffer from poor fracture resistance at low temperatures as well as inadequate creep strength at elevated temperatures. This research program explored macroalloying additions to NiAl-base alloys in order to identify possible alloying and processing routes which promote both low temperature fracture toughness and high temperature strength. Initial results from the study examined the additions of Fe, Co, and Hf on the microstructure, deformation, and fracture resistance of NiAl-based alloys. Of significance were the observations that the presence of the gamma-prime phase, based on Ni3Al, could enhance the fracture resistance if the gamma-prime were present as a continuous grain boundary film or 'necklace'; and the Ni-35Al-20Fe alloy was ductile in ribbon form despite a microstructure consisting solely of the B2 beta phase based on NiAl. The ductility inherent in the Ni-35Al-20Fe alloy was explored further in subsequent studies. Those results confirm the presence of ductility in the Ni-35Al-20Fe alloy after rapid cooling from 750 - 1000 C. However exposure at 550 C caused embrittlement; this was associated with an age-hardening reaction caused by the formation of Fe-rich precipitates. In contrast, to the Ni-35Al-20Fe alloy, exploratory research indicated that compositions in the range of Ni-35Al-12Fe retain the ordered B2 structure of NiAl, are ductile, and do not age-harden or embrittle after thermal exposure. Thus, our recent efforts have focused on the behavior of the Ni-35Al-12Fe alloy. A second parallel effort initiated in this program was to use an alternate processing technique, mechanical alloying, to improve the properties of NiAl-alloys. Mechanical alloying in the conventional sense requires ductile powder particles which, through a cold welding and fracture process, can be dispersion strengthened by submicron-sized oxide particles. Using both the Ni-35Al-Fe alloys to contain approx. 1 v/o Y2O3. Preliminary results indicate that mechanically alloyed and extruded NiAl-Fe + Y2O3 alloys when heat treated to a grain-coarsened condition, exhibit improved creep resistance at 1000 C when compared to NiAl; oxidation resistance comparable to NiAl; and fracture toughness values a factor of three better than NiAl. As a result of the research initiated on this NASA program, a subsequent project with support from Inco Alloys International is underway.

Koss, D. A.↗

Ge{sub 1-y}Sn{sub y} (y = 0.01-0.10) alloys on Ge-buffered Si: Synthesis, microstructure, and optical properties

Novel hydride chemistries are employed to deposit light-emitting Ge{sub 1-y}Sn{sub y} alloys with y ≤ 0.1 by Ultra-High Vacuum Chemical Vapor Deposition (UHV-CVD) on Ge-buffered Si wafers. The properties of the resultant materials are systematically compared with similar alloys grown directly on Si wafers. The fundamental difference between the two systems is a fivefold (and higher) decrease in lattice mismatch between film and virtual substrate, allowing direct integration of bulk-like crystals with planar surfaces and relatively low dislocation densities. For y ≤ 0.06, the CVD precursors used were digermane Ge₂H₆ and deuterated stannane SnD₄. For y ≥ 0.06, the Ge precursor was changed to trigermane Ge₃H₈, whose higher reactivity enabled the fabrication of supersaturated samples with the target film parameters. In all cases, the Ge wafers were produced using tetragermane Ge₄H₁₀ as the Ge source. The photoluminescence intensity from Ge{sub 1–y}Sn{sub y}/Ge films is expected to increase relative to Ge{sub 1–y}Sn{sub y}/Si due to the less defected interface with the virtual substrate. However, while Ge{sub 1–y}Sn{sub y}/Si films are largely relaxed, a significant amount of compressive strain may be present in the Ge{sub 1–y}Sn{sub y}/Ge case. This compressive strain can reduce the emission intensity by increasing the separation between the direct and indirect edges. In this context, it is shown here that the proposed CVD approach to Ge{sub 1–y}Sn{sub y}/Ge makes it possible to approach film thicknesses of about 1 μm, for which the strain is mostly relaxed and the photoluminescence intensity increases by one order of magnitude relative to Ge{sub 1–y}Sn{sub y}/Si films. The observed strain relaxation is shown to be consistent with predictions from strain-relaxation models first developed for the Si{sub 1–x}Ge{sub x}/Si system. The defect structure and atomic distributions in the films are studied in detail using advanced electron-microscopy techniques, including aberration corrected STEM imaging and EELS mapping of the average diamond–cubic lattice.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Conductance control at the LaAlO{sub 3}/SrTiO{sub 3}-interface by a multiferroic BiFeO{sub 3} ad-layer

Multilayered BiFeO{sub 3} (BFO)/LaAlO{sub 3} (LAO) thin film samples were fabricated on SrTiO{sub 3} (STO) substrates by pulsed laser deposition. In this work, the ferroelectric polarization of a multiferroic BFO ad-layer on top of the quasi-two-dimensional electron gas (2DEG) at the LAO/STO interface is used to manipulate the conductivity of the quasi-2DEG. By microstructuring the conductive area of the LAO/STO-interface, a four-point geometry for the measurement of the resistivity was achieved. Piezo force microscopy allows for imaging and poling the spontaneous ferroelectric polarization of the multiferroic layer. The resistance changes showed a linear dependence on the area scanned and a hysteretic behavior with respect to the voltages applied in the scanning process. This is evidence for the ferroelectric polarization of the multiferroic causing the resistance changes. Coupling the antiferromagnetic BFO layer to another ferromagnetic layer could enable a magnetic field control of the conductance of the quasi-2DEG at the LAO/STO interface.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Optimization of L1{sub 0} FePt/Fe{sub 45}Co{sub 55} thin films for rare earth free permanent magnet applications

The magnetic properties of magnetron sputtered bilayers consisting of Fe{sub 45}Co{sub 55} ultrathin layers on top of L1{sub 0} FePt films epitaxially grown on MgO substrates are studied in view of their possible application as rare earth free permanent magnets. It is found that FePt layers induce a tetragonal distortion to the Fe-Co layers which leads to increased anisotropy. This allows to take advantage of the Fe-Co high magnetic moment with less significant loss of the coercivity compared to a typical hard/soft exchange spring system. A maximum energy product approaching 50 MGOe is obtained for a FePt(7 ML)/FeCo/(5 ML) sample. The results are in accordance with first-principles computational methods, which predict that even higher energy products are possible for micromagnetically optimized microstructures.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Correlation Between Microstructure and In-Field Performance of Zr-Added REBCO Coated Conductors Made by Advanced MOCVD

In this paper, we present correlation features between critical current density (J c ) and microstructural characteristics of Zr-added (0, 5, and 15 mol.%) REBa 2 Cu 3 O 7-x (REBCO and RE = rare earth) coated conductors fabricated by the novel advanced metal organic chemical vapor deposition technique. The J c along the tape normal (~ B || c-axis) measured by a vibrating sample magnetometer at 30 and 65 K and magnetic flux density range of 0-14 T was used for qualitative comparison of different Zr-added REBCO tapes. It is found that tapes with enhanced in-field J c exhibit a rise of critical current (plateau or fishtail effect) at magnetic flux density 1-8 T and temperatures 65 K. The TEM microstructure analysis indicates that the plateau effect is not the intrinsic property of REBCO matrix but depends on size distribution and density of BaZrO 3 (BZO) self-assembled nanocolumns. Two types of BZO microstructures have been identified: one with uniform BZO diameter 4-7 nm, whereas some films exhibit bottle-shaped BZO nanocolumns with alternating wide and narrow sections, 7-13 and 4-6 nm, respectively. The non-uniform shape and broad size distribution of BZO nanocolumns are correlated to more vortex pinning strength and matching field.

2G high-temperature superconductor (2GHTS)↗

Thickness-dependent dispersion parameters, energy gap and nonlinear refractive index of ZnSe thin films

Highlights: • Combined experimental and theoretical researches on ZnSe Thin Films. • The film thickness and refractive index were determined using envelope method. • The absorption coefficient and the energy gap were calculated. • Dispersion parameters were determined using Wemple-DiDomenico relation. • The third order susceptibility and nonlinear refractive index were calculated. - Abstract: Zinc selenide (ZnSe) thin films with different thicknesses were evaporated onto glass substrates using the thermal evaporation technique. X-ray diffraction analysis confirmed that both the film and powder have cubic zinc-blende structure. The fundamental optical parameters like absorption coefficient, extinction coefficient and band gap were evaluated in transparent region of transmittance and reflectance spectrum. The optical transition of the films was found to be allowed, where the energy gap increased from 2.576 to 2.702 eV with increasing film thickness. Also, the refractive index value increase with increasing film thickness. The refractive indices evaluated through envelope method were extrapolated by Cauchy dispersion relationship over the whole spectra range. Additionally, the dispersion of refractive index was determined in terms of Wemple-DiDomenico single oscillator model. Third order susceptibility and nonlinear refractive index were determined for different thickness of ZnSe thin films.

36 MATERIALS SCIENCE↗

Effect of substrate temperature on the growth of Nb 3 Sn film on Nb by multilayer sputtering

Here, we report on the fabrication of niobium tin (Nb 3 Sn) films by multilayer sequential sputtering on niobium at substrate temperatures ranging from room temperature to 250 °C. The multilayers were then annealed inside a separate vacuum furnace at 950 °C for 3 h. The material properties of the films were characterized by X-ray diffraction, scanning electron microscopy, energy-dispersive X-ray spectroscopy, atomic force microscopy, and transmission electron microscopy. The superconducting properties of the films were studied by four-point probe resistivity measurements from room temperature to below the superconducting critical temperature T c . The highest film T c was 17.76 K, obtained when the multilayers were deposited at room temperature. When the deposition temperature was raised to 250 °C, a significant reduction in voids was achieved while the film's T c was 17.58 K.

36 MATERIALS SCIENCE↗

Modification of structure and magnetic anisotropy of epitaxial CoFe₂O₄ films by hydrogen reduction

Heteroepitaxial CoFe₂O₄ (CFO) thin films with different thicknesses were deposited on MgO (001) substrates. The as-deposited CFO films show a clear switching of magnetic anisotropy with increasing film thickness. The thinner films (<100 nm) show a perpendicular magnetic anisotropy due to the out-of-plane compressive strain. The thicker films exhibit an in-plane easy axis owing to the dominating shape anisotropy effect. The magnetostriction coefficient of CFO films is estimated to be λ[001] =-188 × 10⁻⁶. Metallic CoFe₂ films were obtained by annealing the as-deposited CFO films in forming gas (Ar 93% + H₂ 7%) at 450 °C. XRD shows that CoFe₂ films are textured out-of-plane and aligned in-plane, owing to lattice matching between CoFe₂ and MgO substrate. TEM results indicate that as-deposited films are continuous while the annealed films exhibit a nanopore mushroom structure. The magnetic anisotropy of CoFe₂ films is dominated by the shape effect. The results demonstrate that hydrogen reduction can be effectively used to modify microstructures and physical properties of complex metal oxide materials.

36 MATERIALS SCIENCE↗

Mechanical response and microprocesses of reconsolidating crushed salt at elevated temperature

Design, analysis and performance assessment of potential salt repositories for heat-generating nuclear waste require knowledge of thermal, mechanical, and fluid transport properties of reconsolidating granular salt. So, to inform salt repository evaluations, we have undertaken an experimental program to determine Bulk and Young’s moduli and Poisson’s ratio of reconsolidated granular salt as a function of porosity and temperature and to establish the deformational processes by which the salt reconsolidates. Our tests were conducted at 100, 175, and 250 °C. In hydrostatic tests, confining pressure is increased to 20 MPa with periodic unload/reload loops to determine K. Volume strain increases with increasing temperature. In shear tests at 2.5 and 5 MPa confining pressure, after confining pressure is applied, the crushed salt is subjected to a differential stress, with periodic unload/reload loops to determine E and ν. At predetermined differential stress levels the stress is held constant and the salt consolidates. Displacement gages mounted on the samples show little lateral deformation until the samples reach a porosity of ~10 %. Interestingly, vapor is vented only for 250 °C tests and condenses at the vent port. It is hypothesized that the brine originates from fluid inclusions, which were made accessible by heating and intragranular deformational processes including decrepitation. Furthermore, identification and documentation of consolidation processes are inferred from optical and scanning electron microstructural observations. As a result, densification at low porosity is enhanced by water film on grain boundaries that enables solution-precipitation phenomena.

58 GEOSCIENCES↗

Asymmetric Cracking in Mar-M247 Alloy Builds During Electron Beam Powder Bed Fusion Additive Manufacturing

In the electron beam powder bed fusion (EB-PBF) process, a substantial number of high-gamma prime Ni-based superalloys are considered as non-printable due to a high propensity to form cracks. In this research, we focused on computational modeling framework to predict solidification-related cracking phenomena in EB-PBF processes. The cracking analysis was performed on cylindrical overhang structures where the cracks are observed only on one side of the part. Comprehensive microstructural characterization correlated the cracking tendency to low-melting point liquid-film formation along columnar grain boundaries with high misorientation angles due to partitioning of alloying elements. Uncoupled numerical thermal and mechanical models were used to rationalize the relationship between process parameters, build geometry, and cracking. The simulations showed asymmetric temperature distributions and associated asymmetric tensile thermal stresses over a cross section due to differences in section modulus and periodic changes in beam scanning directions. Here, the results provide a potential pathway based on spatially varying beam scanning strategies to reduce the cracking tendency during additive manufacturing of complex geometries on the overhang structure in high-gamma prime nickel-based superalloys.

36 MATERIALS SCIENCE↗

Optical waveguiding properties into porous gallium nitride structures investigated by prism coupling technique

In order to modulate the refractive index and the birefringence of Gallium Nitride (GaN), we have developed a chemical etching method to perform porous structures. The aim of this research is to demonstrate that optical properties of GaN can be tuned by controlling the pores density. GaN films are prepared on sapphire by metal organic chemical vapor deposition and the microstructure is characterized by transmission electron microscopy, and scanning electron microscope analysis. Optical waveguide experiment is demonstrated here to determine the key properties as the ordinary (n{sub 0}) and extraordinary (n{sub e}) refractive indices of etched structures. We report here the dispersion of refractive index for porous GaN and compare it to the bulk material. We observe that the refractive index decreases when the porous density p is increased: results obtained at 0.975 μm have shown that the ordinary index n{sub 0} is 2.293 for a bulk layer and n{sub 0} is 2.285 for a pores density of 20%. This value corresponds to GaN layer with a pore size of 30 nm and inter-distance of 100 nm. The control of the refractive index into GaN is therefore fundamental for the design of active and passive optical devices.

36 MATERIALS SCIENCE↗

Thermal Conductivity in Nanocrystalline Ceria Thin Films

The thermal conductivity of nanocrystalline ceria films grown by unbalanced magnetron sputtering is determined as a function of temperature using laser-based modulated thermoreflectance. The films exhibit significantly reduced conductivity compared with stoichiometric bulk CeO2. A variety of microstructure imaging techniques including X-ray diffraction, scanning and transmission electron microscopy, X-ray photoelectron analysis, and electron energy loss spectroscopy indicate that the thermal conductivity is influenced by grain boundaries, dislocations, and oxygen vacancies. The temperature dependence of the thermal conductivity is analyzed using an analytical solution of the Boltzmann transport equation. The conclusion of this study is that oxygen vacancies pose a smaller impediment to thermal transport when they segregate along grain boundaries.

99 GENERAL AND MISCELLANEOUS↗

Electron microscopy study of the microstructure of Ni–W substrate surface

The surface microstructure of Ni–W alloy tapes, which are used as substrates to form films of high-temperature superconductors and photovoltaic devices, has been studied. Several samples of a Ni{sub 95}W{sub 5} tape (Evico) annealed under different conditions were analyzed using scanning electron microscopy, energy-dispersive X-ray microanalysis, electron diffraction, and electron energy-loss spectroscopy. NiWO{sub 4} precipitates are found on the surface of annealed samples. The growth of precipitates at a temperature of 950°C is accompanied by the formation of pores on the surface or under an oxide film. Depressions with a wedge-shaped profile are found at the grain boundaries. Annealing in a reducing atmosphere using a specially prepared chamber allows one to form a surface free of nickel tungstate precipitates.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Solute stabilization of nanocrystalline tungsten against abnormal grain growth

Microstructure and phase evolution in magnetron sputtered nanocrystalline tungsten and tungsten alloy thin films are explored through in situ TEM annealing experiments at temperatures up to 1000 °C. Grain growth in unalloyed nanocrystalline tungsten transpires through a discontinuous process at temperatures up to 550 °C, which is coupled to an allotropic phase transformation of metastable β-tungsten with the A-15 cubic structure to stable body centered cubic (BCC) α-tungsten. Complete transformation to the BCC α-phase is accompanied by the convergence to a unimodal nanocrystalline structure at 650 °C, signaling a transition to continuous grain growth. Alloy films synthesized with compositions of W–20 at.% Ti and W–15 at.% Cr exhibit only the BCC α-phase in the as-deposited state, which indicate the addition of solute stabilizes the films against the formation of metastable β-tungsten. Thermal stability of the alloy films is significantly improved over their unalloyed counterpart up to 1000 °C, and grain coarsening occurs solely through a continuous growth process. The contrasting thermal stability between W–Ti and W–Cr is attributed to different grain boundary segregation states, thus demonstrating the critical role of grain boundary chemistry in the design of solute-stabilized nanocrystalline alloys.

36 MATERIALS SCIENCE↗

Alteration of the UV-visible reflectance spectra of H2O ice by ion bombardment

Satellite in the Jovian and Saturnian system exhibit differences in reflectivity between their 'leading' and 'trailing' surfaces which can affect the local vapor pressure. Since these differences are thought to be due to differences in the flux of bombarding magnetospheric ions, the influence of ion impact on the UV-visible reflectance of water ice surfaces (20-90 K) by keV ion bombardment was studied. An observed decrease in reflectance in the UV is attributed to rearrangement processes that affect the physical microstructure and surface 'roughness'. The ratio in reflectance of bombarded to freshly deposited films is compared to the ratio of the reflectance of the leading and trailing hemispheres for Europa and Ganymede.

Sack, N. J.↗

Passivation and alloying element retention in gas atomized powders

A method for gas atomization of a titanium alloy, nickel alloy, or other alumina (Al.sub.2O.sub.3)-forming alloy wherein the atomized particles are exposed as they solidify and cool in a very short time to multiple gaseous reactive agents for the in-situ formation of a passivation reaction film on the atomized particles wherein the reaction film retains a precursor halogen alloying element that is subsequently introduced into a microstructure formed by subsequent thermally processing of the atomized particles to improve oxidation resistance.

36 MATERIALS SCIENCE↗

Passivation and alloying element retention in gas atomized powders

A method for gas atomization of a titanium alloy, nickel alloy, or other alumina (Al2O3)-forming alloy wherein the atomized particles are exposed as they solidify and cool in a very short time to multiple gaseous reactive agents for the in-situ formation of a passivation reaction film on the atomized particles wherein the reaction film retains a precursor halogen alloying element that is subsequently introduced into a microstructure formed by subsequent thermally processing of the atomized particles to improve oxidation resistance.

36 MATERIALS SCIENCE↗

Passivation and alloying element retention in gas atomized powders

A method for gas atomization of a titanium alloy, nickel alloy, or other alumina (Al 2 O 3 )-forming alloy wherein the atomized particles are exposed as they solidify and cool in a very short time to multiple gaseous reactive agents for the in-situ formation of a passivation reaction film on the atomized particles wherein the reaction film retains a precursor halogen alloying element that is subsequently introduced into a microstructure formed by subsequent thermally processing of the atomized particles to improve oxidation resistance.

Heidloff, Andrew J.↗