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At least 793 records · Page 44

The effect of processing conditions on solidified structures in immiscible systems

The incentive for low-gravity processing of immiscible alloys is usually tied to an attempt to eliminate sedimentation of the more dense immiscible liquid phase during processing. However, many other factors can influence the solidified structure of these alloys. For example, crucible wetting by one of the immiscible liquid phases during normal (non-directional) low-gravity solidification in a container has been shown to often lead to a completely separated structure. For containerless, low-gravity processing, alloy composition has a tremendous affect on the structure formed. During directional solidification, alloy composition, thermal gradient, solidification rate, convective instability and the miscibility gap height of the system all have a major effect on the structures obtained. This paper discusses the conditions necessary for the production of desired microstructures in each of these processing techniques. Examples are shown of samples processed under both desirable and undesirable conditions.

Andrews, J. B.↗

Preparation and Evaluation of Multi-Layer Anodes of Solid Oxide Fuel Cell

The development of an energy device with abundant energy generation, ultra-high specific power density, high stability and long life is critical for enabling longer missions and for reducing mission costs. Of all different types of fuel cells, the solid oxide fuel cells (SOFC) is a promising high temperature device that can generate electricity as a byproduct of a chemical reaction in a clean way and produce high quality heat that can be used for other purposes. For aerospace applications, a power-to-weight of (is) greater than 1.0 kW/kg is required. NASA has a patented fuel cell technology under development, capable of achieving the 1.0 kW/kg figure of merit. The first step toward achieving these goals is increasing anode durability. The catalyst plays an important role in the fuel cells for power generation, stability, efficiency and long life. Not only the anode composition, but its preparation and reduction are key to achieving better cell performance. In this research, multi-layer anodes were prepared varying the chemistry of each layer to optimize the performance of the cells. Microstructure analyses were done to the new anodes before and after fuel cell operation. The cells' durability and performance were evaluated in 200 hrs life tests in hydrogen at 850 C. The chemistry of the standard nickel anode was modified successfully reducing the anode degradation from 40% to 8.4% in 1000 hrs and retaining its microstructure.

Santiago, Diana↗

Mg Isotopic Compositions of Fine-Grained Ca-Al-Rich Inclusions from Reduced CV3 Chondrites and Implications on the Timescale of Nebular Condensation

Fine-grained Ca-Al-rich inclusions (FGIs) in carbonaceous chondrites are interpreted as aggregates of nebular gas-solid condensates that escaped significant melting [1]. Recent Al-Mg isotopic studies of small FGIs (<200 µm in size) from pristine CO3 chondrites have revealed significant variations in initial 26Al/27Al ratio, (26Al/27Al)(sub 0), spanning from 5.73×10(exp ˗5) to 8×10(exp ˗6) [2,3]. Importantly, [3] found a main CAI population characterized by (26Al/27Al)(sub 0) = 5.4×10(exp ˗5) that likely record the onset of dust condensation and initial coagulation events, followed by multiple thermal events over an extended time period. Thus far, a small number of large FGIs from CV3 chondrites have been analyzed, showing a narrower range of ( 26Al/27Al)(sub 0) = 5.27×10(exp ˗5) to 3.35×10(exp ˗5) [4-6], similar to those inferred from coarse-grained, igneous CAIs (CGIs) from CV3 chondrites [7]. These observed different ratios may raise a question if large FGIs in CV3 chondrites record a time interval from primary direct condensation of refractory solids to their aggregation and growth into larger inclusions. In this study, we present Al-Mg isotopic compositions of FGIs from reduced CV3 chondrites to better constrain their formation timescale relative to smaller FGIs in CO3 chondrites, as well as to CGIs in CV3 chondrites. This isotopic study is coordinated with a microstructural study to elucidate the origin and nature of FGIs in the petrologic and mineralogical context.

Han, J.↗

Effects of Microalloying on the Microstructures and Mechanical Properties of Directionally Solidified Ni-33(at.%)Al-31Cr-3Mo Eutectic Alloys Investigated

Despite nickel aluminide (NiAl) alloys' attractive combination of oxidation and thermophysical properties, their development as replacements for superalloy airfoils in gas turbine engines has been largely limited by difficulties in developing alloys with an optimum combination of elevated-temperature creep resistance and room-temperature fracture toughness. Alternatively, research has focused on developing directionally solidified NiAl-based in situ eutectic composites composed of NiAl and (Cr,Mo) phases in order to obtain a desirable combination of properties a systematic investigation was undertaken at the NASA Glenn Research Center to examine the effects of small additions of 11 alloying elements (Co, Cu, Fe, Hf, Mn, Nb, Re, Si, Ta, Ti, and Zr) in amounts varying from 0.25 to 1.0 at.% on the elevated-temperature strength and room-temperature fracture toughness of directionally solidified Ni-33Al-31Cr-3Mo eutectic alloy. The alloys were grown at 12.7 mm/hr, where the unalloyed eutectic base alloy exhibited a planar eutectic microstructure. The different microstructures that formed because of these fifth-element additions are included in the table. The additions of these elements even in small amounts resulted in the formation of cellular microstructures, and in some cases, dendrites and third phases were observed. Most of these elemental additions did not improve either the elevated-temperature strength or the room-temperature fracture toughness over that of the base alloy. However, small improvements in the compression strength were observed between 1200 and 1400 K when 0.5 at.% Hf and 0.25 at.% Ti were added to the base alloy. The results of this study suggest that the microalloying of Ni-33Al-31Cr-3Mo will not significantly improve either its elevatedtemperature strength or its room-temperature fracture toughness. Thus, any improvements in these properties must be acquired by changing the processing conditions.

Whittenberger, J. Daniel↗

Development of sputtered techniques for thrust chambers

Procedures for closing out coolant passages in regeneratively cooled thrust chambers by triode sputtering, using post and hollow Cu-0.15 percent Zr cathodes are described. The effects of aluminum composite filler materials, substrate preparation, sputter cleaning, substrate bias current density and system geometry on closeout layer bond strength and structure are evaluated. High strength closeout layers were sputtered over aluminum fillers. The tensile strength and microstructure of continuously sputtered Cu-0.15 percent Zr deposits were determined. These continuous sputtered deposits were as thick as 0.75 cm. Tensile strengths were consistently twice as great as the strength of the material in wrought form.

Mullaly, J. R.↗

Modeling of Ultrasonically Generated Liquid-Liquid Dispersions During Controlled Directional Solidification

There are innumerable two-component systems in which two very different liquid phases co-exist in equilibrium over a range of temperature and composition, e.g., oil and water, salt fluxes and solders, aluminum and lead. Often it is of practical concern to fabricate a solid component consisting of a uniform dispersion of one phase in the other. Unfortunately, uniform microstructural development during solidification of two immiscible liquids is hampered by inherent, often large, density differences between the phases that lead to severe segregation. Uniformity is also compromised by preferential wetting and coalescence phenomena. It is, however, well known that ultrasonic energy can initiate and maintain a fine liquid-liquid dispersion. The work presented here extends that observation by application of ultrasonic energy to promote uniform phase incorporation during controlled directional solidification. To this end experiments with the transparent organic, immiscible, succinonitrile-glycerol system were conducted and the numerous processing parameters associated with this technique were evaluated in view of optimizing dispersion uniformity. In view of the initial experimental results a model that predicts the dispersed liquid droplet size as a function of material properties, sample geometry, and applied energy has been developed. In the mathematical model we consider the ultrasonic field in an experimental ampoule of length L and diameter D induced by a probe having a vibration frequency of f=2OKhz (circular frequency omega = 2 pi f). The amplitude is adjustable from A=65 to 13Omicrons. The probe tip diameter is d, the liquid has a density of p, in which the speed of sound and surface tension are, respectively, c and sigma. The mathematical model and numerical investigation for the experiments [1] is done using the following assumptions: (i) The droplet size is small in comparison to the sound wave length; (ii) The forces between droplets are neglected (relative concentration is small); (iii) The droplet is stable if the kinetic energy, E(sub K), of the liquid motion due to ultrasonic field influence is less then the binding energy, E(sub S), due to the surface tension (it is easy to show that the surface energy of two droplets resulting from one is larger by about a factor of two.); (iv) The stability limit is characterized by E(sub S) to approx. E(sub K).

Grugel, R. N.↗

Development of Ceramic Systems for High temperature Coatings

Professor Eslamloo-Grami will synthesize ceramic powders of various compositions based on pyrochlore, perovskite, and magnetoplumbite structures by doping with various oxides. Sol-gel and combustion synthesis routes will be used for powder syntheses. The powders will be characterized for particle size, surface area, microstructure, sintering etc. Thermal conductivity of the hot pressed specimens will also be measured at various temperatures. At the end, a project report will be prepared describing in details the experimental methods, results, discussion, and future research.

Eslamloo-Grami, Maryame↗

Lunar and Planetary Science XXXV: Lunar Sample Analysis

The titles in this section include: 1) Global Mixing as a Mechanism for Compositional Anomalies of Agglutinitic Glasses; 2) Electron Microscopy of Apollo 12 Glass Spherules; 3) 40Ar-39Ar Geochronology on Apollo 12 Regolith; 4) LSCC Apollo and Luna Soil Analyses: Update of Soil Evolution Model; 5) Planetary Regolith Microstructure: An Unexpected Opposition Effect Result; 6) Infrared Spectroscopy on a Microscopic Scale: Investigating the Technique of Microspectroscopy and Its Application to a Lunar Breccia; 7) The Most Reduced Rock from the Moon - Apollo 14 Basalt 14053: Extreme Reduction Entirely from a Re-Heating Event.

Source record↗

Adhesive Bonding of Titanium to Carbon-Carbon Composites for Heat Rejection Systems

High temperature adhesives with good thermal conductivity, mechanical performance, and long term durability are crucial for the assembly of heat rejection system components for space exploration missions. In the present study, commercially available adhesives were used to bond high conductivity carbon-carbon composites to titanium sheets. Bonded pieces were also exposed to high (530 to 600 Kelvin for 24 hours) and low (liquid nitrogen 77K for 15 minutes) temperatures to evaluate the integrity of the bonds. Results of the microstructural characterization and tensile shear strengths of bonded specimens will be reported. The effect of titanium surface roughness on the interface microstructure will also be discussed.

Cerny, Jennifer↗

Particle Morphology and Elemental Composition of Smoke Generated by Overheating Common Spacecraft Materials

Fire safety in the indoor spacecraft environment is concerned with a unique set of fuels which are designed to not combust. Unlike terrestrial flaming fires, which often can consume an abundance of wood, paper and cloth, spacecraft fires are expected to be generated from overheating electronics consisting of flame resistant materials. Therefore, NASA prioritizes fire characterization research for these fuels undergoing oxidative pyrolysis in order to improve spacecraft fire detector design. A thermal precipitator designed and built for spacecraft fire safety test campaigns at the NASA White Sands Test Facility (WSTF) successfully collected an abundance of smoke particles from oxidative pyrolysis. A thorough microscopic characterization has been performed for ten types of smoke from common spacecraft materials or mixed materials heated at multiple temperatures using the following techniques: SEM, TEM, high resolution TEM, high resolution STEM and EDS. Resulting smoke particle morphologies and elemental compositions have been observed which are consistent with known thermal decomposition mechanisms in the literature and chemical make-up of the spacecraft fuels. Some conclusions about particle formation mechanisms are explored based on images of the microstructure of Teflon smoke particles and tar ball-like particles from Nomex fabric smoke.

Smoke↗

High-temperature strength of refractory-metal wires and consideration for composite applications

Tensile and stress-rupture tests were conducted on wires of W-Hf-C, W-Re-Hf-C, ASTAR 811C (a tantalum alloy), and B-88 (a columbium alloy) at room temperature, 1093 C (2000 F), and 1204 C (2200 F). Metallographic examinations were also made of the wire microstructure after testing. Ultimate tensile strength values up to 2170 meganewtons per square meter (314000 psi) at 1093 C (2000 F) and 1940 meganewtons per square meter (281 000 psi) at 1204 C (2200 F) were obtained for W-Re-Hf-C wire. The best strength values obtained for a 100-hour rupture life were, 1410 meganewtons per square meter (205 000 psi) at 1093 C (2000 F) and 910 meganewtons per square meter (132 000 psi) at 1240 C (2200 F) for W-Re-Hf-C wire. The properties obtained suggested that the wires studied showed promise as potential fiber reinforcement in the 1093 to 1204 C (2000 to 2200 F) temperature range.

Petrasek, D. W.↗

Determination of the Fe-Ni phase diagram below 400 C

Analytical EM techniques have been used to obtain a phase diagram for the Fe-Ni system below 400 C in the composition range from 0-52 wt pct Ni. The present diagram is consistent with all the phases observed in the Fe-Ni regions of meteorites. An asymmetric spinodal decomposition results in the expected two-phase isotropic microstructure. The present experimentally-determined miscibility gap below 400 C, located between 11.7 and 51.9 wt pct Ni at 200 C, is shown to be wider than the calculated miscibility gap.

Reuter, K. B.↗

Containerless, Low-Gravity Undercooling of Ti-Ce Alloys in the MSFC Drop Tube

Previous tests of the classical nucleation theory as applied to liquid-liquid gap miscibility systems found a discrepancy between experiment and theory in the ability to undercool one of the liquids before the L1-L2 separation occurs. To model the initial separation process in a two-phase liquid mixture, different theoretical approaches, such as free-energy gradient and density gradient theories, have been put forth. If there is a large enough interaction between the critical liquid and the crucible, both models predict a wetting temperature (T(sub w)) above which the minority liquid perfectly wets and layers the crucible interface, but only on one side of the immiscibility dome. Materials with compositions on the other side of the dome will have simple surface adsorption by the minority liquid before bulk separation occurs when the coexistence (i.e., binoidal) line in reached. If the interaction between the critical liquid and the crucible were to decrease, T(sub w) would increase, eventually approaching the critical consolute temperature (T(sub cc)). If this situation occurs, then there could be large regions of the miscibility gap where non-perfect wetting conditions prevail resulting in droplets of L1 liquid at the surface having a non-zero contact angle. The resulting bulk structure will then depend on what happens on the surface and the subsequent processing conditions. In the past several decades, many experiments in space have been performed on liquid metal binary immiscible systems for the purpose of determining the effects that different crucibles may have on the wetting and separation process of the liquids. Potard performed experiments that showed different crucible materials could cause the majority phase to preferentially wet the container and thus produce a dispersed microstructure of the minority phase. Several other studies have been performed on immiscibles in a semi-container environment using an emulsion technique. Only one previous study was performed using completely containerless processing of immiscible metals and the results of that investigation are similar to some of the emulsion studies. In all the studies, surface wetting was attributed as the cause for the similar microstructures or the asymmetry in the ability to undercool the liquid below the binoidal on one side of the immiscibility dome. By removing the container completely from the separation process, it was proposed that the loss of the crucible/liquid interaction would produce a large shift in T(sub w) and thus change the wetting characteristics at the surface. By investigating various compositions across the miscibility gap, a change in the type and amount of liquid wetting at the surface of a containerless droplet should change the surface nucleating behavior of the droplet - whether it be the liquid-liquid wetting or the liquid-to-solid transition. Undercooling of the liquid into the metastable region should produce significant differences in the separation process and the microstructure upon solidification. In this study, we attempt to measure these transitions by monitoring the temperature of the sample by optical pyrometry. Microstructural analysis will be made to correlate with the degree of undercooling and the separation mechanisms involved.

Robinson, M. B.↗

Mechanical, Chemical and Microstructural Characterization of Monazite-Coated Silicon Carbide Fibers

Tensile strengths of as-received Hi-Nicalon and Sylramic fibers and those having monazite surface coatings, deposited by atmospheric pressure chemical vapor deposition, were measured at room temperature and the Weibull statistical parameters determined. The average tensile strengths of uncoated Hi-Nicalon and Sylramic fibers were 3.19 +/- 0.73 and 2.78 +/- 0.53 GPa with a Weibull modulus of 5.41 and 5.52, respectively. The monazite-coated Hi-Nicalon and Sylramic fibers showed strength loss of approx. 10 and 15 percent, respectively, compared with the as-received fibers. The elemental compositions of the fibers and the coatings were analyzed using scanning Auger microprobe and energy dispersive X-ray spectroscopy. The LaPO4 coating on Hi-Nicalon fibers was approximately stoichiometric and about 50 nm thick. The coating on the Sylramic fibers extended to a depth of about 100 to 150 nm. The coating may have been stoichiometric LaPO4 in the first 30 to 40 nm of the layer. However, the surface roughness of Sylramic fiber made this profile somewhat difficult to interpret. Microstructural analyses of the fibers and the coatings were done by scanning electron microscopy, transmission electron microscopy, and selected area electron diffraction. Hi-Nicalon fiber consists of fine beta-SiC nanocrystals ranging in size from 1 to 30 mn embedded in an amorphous matrix. Sylramic is a polycrystalline stoichiometric silicon carbide fiber consisting of submicron beta-SiC crystallites ranging from 100 to 300 nm. Small amount of TiB2 nanocrystallites (approx. 50 nm) are also present. The LaPO4 coating on Hi-Nicalon fibers consisted of a chain of peanut shape particles having monazite-(La) structure. The coating on Sylramic fibers consisted of two layers. The inner layer was a chain of peanut shape particles having monazite-(La) structure. The outer layer was comprised of much smaller particles with a microcrystalline structure.

Bansal, N. P.↗

Effect of polymer properties and adherend surfaces on adhesion

High temperature polymer surface characteristics associated with joint strength were evaluated. Selected samples represented composite adherends, aluminum filler and fiber glass carrier cloth. Detailed analysis of fractured joint surfaces revealed unique characteristics typical of the specific adhesive formulations and test conditions. A fracture mechanism model was developed for correlating macroscopic shear strength and microstructure of fracture surfaces. Applications were made to unpublished data on polyimides and fluoropolymers.

Dwight, D. W.↗

Strength and microstructure of Si3N4 sintered with ZrO2 additions

Densities greater than 99 percent of theoretical were obtained with stabilized ZrO2 additions to Si3N4. Material sintered at 2140 C under 2.5 MPa nitrogen overpressure with 3.8, 9.9, and 13.4 wt pct ZrO2 had a predominantaly equiaxed grain size ranging from 0.2 to 7.0 microns. At 1370 C, the latter composition exhibited a flexural strength of about 487 MPa, equal to that of a finer-grain-size, hot-pressed Si3N4 + ZrO2 material having excellent high-temperature static fatigue properties. Transmission electron microscopy of the sintered Si3N4 revealed a glassy grain-boundary phase at all three ZrO2 levels and partially crystalline triple points for the 9.9 and 13.4 wt pct ZrO2-containing materials. Slow crack growth was observed for 1370 C flexure tests and correlated with nonlinear load deflection traces for stresses greater than 503 MPa. The crystallization of the grain-boundary glass is insterpreted as beneficial to the attainment of high (1370 C) flexural strength.

Sanders, W. A.↗

Mullite Whiskers and Mullite-whisker Felt

The Naval Surface Warfare Center has developed processes for the preparation of mullite (3(Al2O3)(dot)2(SiO2)) whiskers and mullite-whisker felt. Three patents on the technology were issued in 1990. The processes are based on chemical reactions between AlF3, Al2O3, and SiO2. The felt is formed in-situ during the processing of shaped powdered precursors. It consists of randomly oriented whiskers which are mutually intergrown forming a rigid structure. The microstructure and properties of the felt and size of the whiskers can be modified by varying the amount of Al2O3 in the starting mixture. Loose mullite whiskers can be used as a reinforcement for polymer-, metal-, and ceramic-matrix composites. The felt can be used as preforms for fabricating composite materials as well as for thermal insulation and high temperature, chemically stable filters for liquids (melts) and gases.

Talmy, Inna G.↗

An analytical/numerical correlation study of the multiple concentric cylinder model for the thermoplastic response of metal matrix composites

The utility of a recently developed analytical micromechanics model for the response of metal matrix composites under thermal loading is illustrated by comparison with the results generated using the finite-element approach. The model is based on the concentric cylinder assemblage consisting of an arbitrary number of elastic or elastoplastic sublayers with isotropic or orthotropic, temperature-dependent properties. The elastoplastic boundary-value problem of an arbitrarily layered concentric cylinder is solved using the local/global stiffness matrix formulation (originally developed for elastic layered media) and Mendelson's iterative technique of successive elastic solutions. These features of the model facilitate efficient investigation of the effects of various microstructural details, such as functionally graded architectures of interfacial layers, on the evolution of residual stresses during cool down. The available closed-form expressions for the field variables can readily be incorporated into an optimization algorithm in order to efficiently identify optimal configurations of graded interfaces for given applications. Comparison of residual stress distributions after cool down generated using finite-element analysis and the present micromechanics model for four composite systems with substantially different temperature-dependent elastic, plastic, and thermal properties illustrates the efficacy of the developed analytical scheme.

Pindera, Marek-Jerzy↗