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All sourcesNASA NTRSDOE OSTI
NASA NTRS1995

High-Temperature Oxidation Behavior of Iridium-Rhenium Alloys

The life-limiting mechanism for radiation-cooled rockets made from iridium-coated rhenium (Ir/Re) is the diffusion of Re into the Ir layer and the subsequent oxidation of the resulting Ir-Re alloy from the inner surface. In a previous study, a life model for Ir/Re rockets was developed. It incorporated Ir-Re diffusion and oxidation data to predict chamber lifetimes as a function of temperature and oxygen partial pressure. Oxidation testing at 1540 deg C suggested that a 20-wt percent Re concentration at the inner wall surface should be established as the failure criterion. The present study was performed to better define Ir-oxidation behavior as a function of Re concentration and to supplement the data base for the life model. Samples ranging from pure Ir to Ir-40 wt percent Re (Ir-40Re) were tested at 1500 deg C, in two different oxygen environments. There were indications that the oxidation rate of the Ir-Re alloy increased significantly when it went from a single-phase solid solution to a two-phase mixture, as was suggested in previous work. However, because of testing anomalies in this study, there were not enough dependable oxidation data to definitively raise the Ir/Re rocket failure criterion from 20-wt percent Re to a Re concentration corresponding to entry into the two-phase region.

Reed, Brian D.↗
NASA NTRS1994

A new titanium-bearing calcium aluminosilicate phase. 2: Crystallography and crystal chemistry of grains formed in slowly cooled melts with bulk compositions of calcium-aluminium-rich inclusions

The crystallography and crystal chemistry of a new calcium- titanium-aluminosilicate mineral (UNK) observed in synthetic analogs to calcium-aluminum-rich inclusions (CAIs) from carbonaceous chondrites was studied by electron diffraction techniques. The unit cell is primitive hexagonal or trigonal, with a = 0.790 +/- 0.02 nm and c = 0.492 +/- 0.002 nm, similar to the lattice parameters of melilite and consistent with cell dimensions for crystals in a mixer furnace slag described by Barber and Agrell (1994). The phase frequently displays an epitactic relationship in which melilite acts as the host, with (0001)(sub UNK) parallel (001)(sub mel) and zone axis group 1 0 -1 0(sub UNK) parallel zone axis group 1 0 0(sub mel). If one of the two space groups determined by Barber and Agrell (1994) for their sample of UNK is applicable (P3m1 or P31m), then the structure is probably characterized by puckered sheets of octahedra and tetrahedra perpendicular to the c-axis with successive sheets coordinated by planar arrays of Ca. In this likely structure, each unit cell contains three Ca sites located in mirror planes, one octahedrally coordinated cation located along a three-fold axis and five tetrahedrally coordinated cations, three in mirrors and two along triads. The octahedron contains Ti but, because there are 1.3-1.9 cations of Ti/formula unit, some of the Ti must also be in tetrahedral coordination, an unusual but not unprecedented situation for a silicate. Tetrahedral sites in mirror planes would contain mostly Si, with lesser amounts of Al while those along the triads correspondingly contain mostly Al with subordinate Ti. The structural formula, therefore, can be expressed as Ca(sub 3)(sup VIII)(Ti,Al)(sup VI)(Al,Ti,Si)(sub 2)(sup IV)(Si,Al)(sub 3)(sup IV)O14 with Si + Ti = 4. Compositions of meteoritic and synthetic Ti-bearing samples of the phase can be described in terms of a binary solid solution between the end-members Ca3TiAl2Si3O14 and Ca3Ti(AlTi)(AlSi2)O14. A Ti-free analog with a formula of Ca3Al2Si4O14 synthesized by Paque et al. (1994) is thought to be related structurally but with the octahedral site being occupied by Al, that is, Ca(sub 3)(sup VIII)Al(sup VI)(Al,Si)(sub 2)(sup IV)(Si)(sub 3)(sup IV)O14.

Barber, David J.↗
NASA NTRS1991

High rate reactive sputtering of MoN(x) coatings

High rate reactive sputtering of MoN(x) films was performed using feedback control of the nitorgen partial pressure. Coatings were made at four different target powers: 2.5, 5.0, 7.5 and 10 kW. No hysteresis was observed in the nitrogen partial pressure vs. flow plot, as is typically seen for the Ti-N system. Four phases were determined by X-ray diffraction: molybdenum, Mo-N solid solution, Beta-Mo2N and gamma-Mo2N. The hardness of the coatings depended upon composition, substrate bias, and target power. The phases present in the hardest films differed depending upon deposition parameters. For example, the Beta-Mo2N phase was hardest (load 25 gf) at 5.0 kW with a value of 3200 kgf/sq mm, whereas the hardest coatings at 10 kW were the gamma-Mo2N phase (3000 kgf/sq mm). The deposition rate generally decreased with increasing nitrogen partial pressure, but there was a range of partial pressures where the rate was relatively constant. At a target power of 5.0 kW, for example, the deposition rates were 3300 A/min for a N2 partial pressure of 0.05 - 1.0 mTorr.

Rudnik, Paul J.↗
NASA NTRS1994

The stability of hibonite, melilite and other aluminous phases in silicate melts: Implications for the origin of hibonite-bearing inclusions from carbonaceous chondrites

Phase fields in which hibonite and silicate melt coexist with spinel CaAl4O7, gehlenitic melilite, anorthite or corundum at 1 bar in the system CaO-MgO-Al2O3-SiO2-TiO2 were determined. The hibonites contain up to 1.7 wt% SiO2. For TiO2, the experimentally determined partition coefficients between hibonite and coexisting melt D(sub i)(sup Hib/L), vary from 0.8 to 2.1 and generally decrease with increasing TiO2 in the liquid. Based on Ti partitioning between hibonite and melt, bulk inclusion compositions and hibonite-saturated liquidus phase diagrams, the hibonite in hibonite-poor fluffy Type A inclusions from Allende and at least some hibonite from hibonite-rich inclusions is relict, although much of the hibonite from hibonite-glass spherules probably crystallized metasably from a melt. Bulk compositions for all of these CAIs are consistent with an origin as melite + hibonite + spinel + perovskite phase assembalges that were partially altered and in some cases partially or completely melted. The duration of the melting event was sufficient to remove any Na introduced by the alteration process but frequently insufficient to dissolve all of the original hibonite. Simple thermochemical models developed for meteoritic melilite and hibonite solid solutions were used to obtain equilibration temperatures of hibonite-bearing phase assemblages with vapor. Referenced to 10(exp -3) atm, hibonite + corundum + vapor equilibrated at approximately 1260 C and hibonite + spinel +/- melilite + vapor at 1215 +/- 10 C. If these temperatures reflect condensation in a cooling gas of solar composition, then hibonite +/- corundum condensed first, followed by spinel and then melilite. The position of perovskite within this sequence is uncertain, but it probably began to condense before spinel. This sequence of phase appearances and relative temperatures is generally consistent with observed textures but differs from expectations based on classical condensation calculations in that equilibration temperatures are generally lower than predicted and melilite initially condenses with or even after spinel. Simple thermochemical modes for the substitution of trace elements into the Ca site of meteoritic hibonites suggest that virtually all Eu is divalent in early condensate hibonites but that Eu(2+)/Eu(#+) decreases by a factor of 20 or more during the course of condensation primarily because the ratio is proportional to the partial pressure of Al, which decreases dramatically as aluminous phase condense. The relative sizes of Eu and Yb anomalies in meteoritic hibonites and inclusions may be partly due to this effect.

Beckett, J. R.↗
NASA NTRS1994

Occurence and implications of silicon nitride in enstatic chondrites

Silicon nitride Si3N4, has previously been observed to be a common constituent of acid residues of Qingzhen (EH3) and Indarch (EH4). Ion probe analysis of the Si, N and C isotopic compositions of individual Si3N4 grains from Qingzhen and Indarch acid residues suggest most, if not all, grains are Solar System in origin. A few grains have isotopically anomalous C but this is probably due to small presolar SiC grains adhering to them. In situ observations of the Si3N4 in Qingzhen show that it is only present within, and probably exsolved from, host phases which contain elemental Si in solid solution. Thermodynamic calculations suggest that the Si3N4 probably formed during metamorphism and not in the nebula. Thermodynamic calculations also show that sinoite (Si2N2O) and not Si3N4 should be the stable phase during metamorphism. It appears that kinetic factors must have inhibited the formation if sinoite in Qimgzhen and Indarch.

Alexander, C. M. O'D.↗
NASA NTRS1995

Oxide perovskite crystals for HTSC film substrates microwave applications

The research focused upon generating new substrate materials for the deposition of superconducting yttrium barium cuprate (YBCO) has yielded several new hosts in complex perovskites, modified perovskites, and other structure families. New substrate candidates such as Sr(Al(1/2)Ta(1/2))O3 and Sr(Al(1/2)Nb(1/2))O3, Ba(Mg(1/3)Ta(2/3))O3 in complex oxide perovskite structure family and their solid solutions with ternary perovskite LaAlO3 and NdGaO3 are reported. Conventional ceramic processing techniques were used to fabricate dense ceramic samples. A laser heated molten zone growth system was utilized for the test-growth of these candidate materials in single crystal fiber form to determine crystallographic structure, melting point, thermal, and dielectric properties as well as to make positive identification of twin free systems. Some of those candidate materials present an excellent combination of properties suitable for microwave HTSC substrate applications.

Bhalla, A. S.↗
NASA NTRS1996

Skutterudite Compounds For Power Semiconductor Devices

New semiconducting materials with p-type carrier mobility values much higher than state-of-art semiconductors discovered. Nine compounds, antimonides CoSb(sub3), RhSb(sub3), IrSb(sub3), arsenides CoAs(sub3), RhAs(sub3), IrAs(sub3), and phosphides CoP(sub3), RhP(sub3) and IrP(sub3), exhibit same skutterudite crystallographic structure and form solid solutions of general composition Co(1-x-y)RH(x)Ir(y)P(1-w-z)As(w)Sb(z). Materials exhibit high hole mobilities, high doping levels, and high electronic figures of merit. Some compositions show great potential for application to thermoelectric devices.

Fleurial, Jean-Pierre↗
NASA NTRS1995

Positron annihilation spectroscopic study of high performance semi-interpenetrating network polyimids

Semi-interpenetrating (S-IPN) network polyimids were made from different proportions of LaRC RP46 (a thermosetpolyimid) and LaRC BDTA-ODA (a thermoplastic polyimid). The ultimate goal of this networking is to improve the mechanical properties of the thermoset polyimid. Positron lifetime study was made to calculate lifetime based on second component of the life time spectra and the free volume & microvoid size. All these properties tend to decrease steadily with increasing thermoset content except at the 50 percent thermoset level where these properties show sudden drop. This result contradicts with the initial expectation that the blend properties should change gradually if it were a solid solution of thermoset (TSP) and thermoplastic (TPP) components. Thermal analyses (TMA, DSC, DMA & TGA) were run to complement the positron life time studies. The TMA and DSC studies confirm the contradiction mentioned above. Further experimentation with S-IPN polymers made at TSP/TTP content around 50/50 level are being conducted to explain this anomaly. Scanning electron microscope study of the S-IPN polyimid samples is under way in order to detect morphological differences which might help explain the phenomenon mentioned above.

Ray, Asit K.↗
NASA NTRS1996

High temperature coarsening of Cr2Nb precipitates in Cu-8 Cr-4 Nb alloy

A new high-temperature-strength, high-conductivity Cu-Cr-Nb alloy with a CrNb ratio of 2:1 was developed to achieve improved performance and durability. The Cu-8 Cr4 Nb alloy studied has demonstrated remarkable thermal and microstructural stability after long exposures at temperatures up to 0.98 T(sub m). This stability was mainly attributed to the slow coarsening kinetics of the Cr2Nb precipitates present in the alloy. At all temperatures, the microstructure consists of a bimodal and sometimes trimodal distribution of strengthening Cr2Nb precipitates, depending on precipitation condition, i.e. from liquid or solid solution, and cooling rates. These precipitates remain in the same size range, i.e. large precipitates of approximately I pm, and small precipitates less dm 300 nm, and effectively pin the grain boundaries thus retaining a fine grain size of 2.7 micro-m after 100 h at 1323 K. (A relatively small number of Cr-rich and Nb-rich particles were also present.) This grain boundary pinning and sluggish coarsening of Cr2Nb particles explain the retention of good mechanical properties after prolonged holding at very high temperatures, e.g., 75% of the original hardness after aging for 100 h at 1273 K. Application of LSW-based coarsening models indicated that the coarsening kinetics of the large precipitates are most likely governed by grain boundary diffsion and, to a lesser extent, volume diffusion mechanisms.

Anderson, Kenneth Reed↗
NASA NTRS1996

Microstructural Characterization of Semi-Interpenetrating Polymer Networks by Positron Lifetime Spectroscopy

Thermoset and thermoplastic polyimides have complementary physical and mechanical properties. Whereas thermoset polyimides are brittle and generally easier to process, thermoplastic polyimides are tough but harder to process. A combination of these two types of polyimides may help produce polymers more suitable for aerospace applications. Semi-Interpenetrating Polymer Networks (S-IPN) of thermoset LaRC(TM)-RP46 and thermoplastic LaRC(TM)-IA polyimides were prepared in weight percent ratios ranging from 100:0 to 0:100. Positron lifetime measurements were made in these samples to correlate their free volume features with physical and mechanical properties. As expected, positronium atoms are not formed in these samples. The second lifetime component has been used to infer the positron trap dimensions. The 'free volume' goes through a minimum at a ratio of about 50:50, and this suggests that S-IPN samples are not merely solid solutions of the two polymers. These data and related structural properties of the S-IPN samples are discussed.

Singh, Jag J.↗
NASA NTRS1997

Low Temperature Synthesis, Chemical and Electrochemical Characterization of LiNi(x)Co(1-x)O2 (0 less than x less than 1)

A new method of synthesis for the solid solution cathode materials LiNi(x)Co(1-x)O2 (0 less than x less than 1) involving enhanced reactions at temperatures less than or equal to 700 deg. C, between metal oxy-hydroxide precursors MOOH (M = Ni, Co) and Li-salts (Li2CO3, LiOH, and LiNO3) has been investigated. The effects of synthesis conditions and sources of Li, on phase purity, microstructure, and theoretical electrochemical capacity (total M(3+) content) are characterized by powder X-ray diffraction analysis, scanning electron microscopy, chemical analysis and room temperature magnetic susceptibility. An attempt has been made to correlate the electrochemical properties with the synthesis conditions and microstructure.

Nanjundaswamy, K. S.↗
NASA NTRS1996

Directional Solidification of Mercury Cadmium Telluride During the Second United States Microgravity Payload Mission (USMP-2)

As a solid solution semiconductor having, a large separation between liquidus and solidus, mercury cadmium telluride (MCT) presents a formidable challenge to crystal growers desiring an alloy of high compositional uniformity. To avoid constitutional supercooling during Bridgman crystal growth it is necessary to solidify slowly in a high temperature gradient region. The necessary translation rate of less than 1 mm/hr results in a situation where fluid flow induced by gravity on earth is a significant factor in material transport. The Advanced Automated Directional Solidification Furnace (AADSF) is equipped to provide the stable thermal environment with a high gradient, and the required slow translation rate needed. Ground based experiments in AADSF show clearly the dominance of flow driven transport. The first flight of AADSF in low gravity on USMP-2 provided an opportunity to test theories of fluid flow in MCT and showed several solidification regimes which are very different from those observed on earth. Residual acceleration vectors in the orbiter during the mission were measured by the Orbital Acceleration Research Experiment (OARE), and correlated well with observed compositional differences in the samples.

Gillies, D. C.↗
NASA NTRS1994

Elevated-Temperature Deformation Properties of a HfC Modified Ti-48Al-2Mn-2Nb Matrix Particulate Composite

Rapid solidification techniques in combination with HIPing have been used to produce Ti-48Al-2Mn-2Nb and a Ti-48Al-2Mn-2Nb+15 wt% HfC composite. While the composite does contain several second phases within the gamma + alpha(sub 2) matrix, none was identified to be HfC. The elevated-temperature properties were determined by constant velocity compression and constant load tensile testing in air between 1000 and 1173 K. Such testing indicated that the elevated temperature strengths of the HfC-modified aluminide was superior to those of the unreinforced matrix with the best 1100 K temperature slow strain rate properties for both materials being achieved after high-temperature annealing prior to testing. Examination of the microstructures after deformation in combination with the measured stress exponents and activation energies suggest that creep resistance of the HfC-modified form is due to solid-solution strengthening from carbon and hafnium rather than the presence of second phases.

Whittenberger, J. D.↗
NASA NTRS1997

Contact Sensor Attachment to Titanium Metal Composites

A Pd-13wt%Cr solid solution is a promising high-temperature strain gage alloy. In bulk form it has a number of properties that are desirable in a resistance strain gage material, such as a linear electrical-resistance-versus-temperature curve to 1000 C and stable electrical resistance in air at 1000 C. However, unprotected fine wire gages fabricated from this alloy perform well only to 600 C. At higher temperatures severe oxidation degrades their electrical performance. In this work Auger electron spectroscopy has been used to study the oxidation chemistry of the alloy wires and ribbons. Results indicate that the oxidation is caused by a complex mechanism that is not yet fully understood. As expected, during oxidation, a layer of chromium oxide is formed. This layer, however, forms beneath a layer of metallic palladium. The results of this study have increased the understanding of the oxidation mechanism of Pd-13wt%Cr.

Vargas-Aburto, Carlos↗
NASA NTRS1998

The Effect of Alloying on Topologically Close Packed Phase Instability in Advanced Nickel-Based Superalloy Rene N6

An investigation was conducted to describe topologically close packed (TCP) phase instability as a function of composition in the advanced Ni-base superalloy Rene N6. TCP phases are detrimental to overall high-temperature performance of Ni-base superalloys because of their brittle nature and because they deplete the Ni-rich matrix of potent solid solution strengthening elements. Thirty-four variations of polycrystalline Rene N6 determined from a design-of-experiments approach were cast and homogenized at 1315"C for 80 hours followed by exposure at 10930C for 400 hours to promote TCP formation. The alloys had the following composition ranges in atomic percent: Co 10.61 to 16.73%, Mo 0.32 to 1.34%, W 1.85 to 2.52%, Re 1.80 to 2.1 1 %, Ta 2.36 to 3.02%, Al 11.90 to 14.75%, and Cr 3.57 to 6.23%. Physical and chemical characteristics of all n-ticrostructures obtained were described using various analytical techniques. From these observations, a mathematical description of TCP occurrence (omega and P phase) was generated for polycrystalline Rene N6.

Ritzert, Frank↗
NASA NTRS1998

Nuclear Instruments and Methods in Physics Research: Microstructural Characterization of Semi-Interpenetrating Polymer Networks by Positron Lifetime Spectroscopy - Section B

Thermoset and thermoplastic polyimides have complementary physical/mechanical properties. Whereas thermoset polyimides are brittle and generally easier to process, thermoplastic polyimides are tough but harder to process. It is expected that a combination of these two types of polyimides may help produce polymers more suitable for aerospace applications. Semi-Interpenetrating Polymer Networks (S-IPNs) of thermoset LaRC(Trademark)-RP46 and thermoplastic LARC(Trademark)-IA polyimides were prepared in weight percent ratios ranging from 100:0 to 0: 100. Positron lifetime measurements were made in these samples to correlate their free volume features with physical/mechanical properties. As expected, positronium atoms are not formed in these samples. The second life time component has been used to infer the positron trap dimensions. The "free volume" goes through a minimum at about 50:50 ratio, suggesting that S-IPN samples are not merely solid solutions of the two polymers. These data and related structural properties of the S-IPN samples have been discussed in this paper.

Singh, Jag J.↗
NASA NTRS1999

Crystal Growth of II-VI Semiconducting Alloys by Directional Solidification

This research study is investigating the effects of a microgravity environment during the crystal growth of selected II-VI semiconducting alloys on their compositional, metallurgical, electrical and optical properties. The on-going work includes both Bridgman-Stockbarger and solvent growth methods, as well as growth in a magnetic field. The materials investigated are II-VI, Hg(1-x)Zn(x)Te, and Hg(1-x)Zn(x)Se, where x is between 0 and 1 inclusive, with particular emphasis on x-values appropriate for infrared detection and imaging in the 5 to 30 micron wavelength region. Wide separation between the liquidus and solidus of the phase diagrams with consequent segregation during solidification and problems associated with the high volatility of one of the components (Hg), make the preparation of homogeneous, high-quality, bulk crystals of the alloys an extremely difficult nearly an impossible task in a gravitational environment. The three-fold objectives of the on-going investigation are as follows: (1) To determine the relative contributions of gravitationally-driven fluid flows to the compositional redistribution observed during the unidirectional crystal growth of selected semiconducting solid solution alloys having large separation between the liquidus and solidus of the constitutional phase diagram; (2) To ascertain the potential role of irregular fluid flows and hydrostatic pressure effects in generation of extended crystal defects and second-phase inclusions in the crystals; and, (3) To obtain a limited amount of "high quality" materials needed for bulk crystal property characterizations and for the fabrication of various device structures needed to establish ultimate material performance limits. The flight portion of the study was to be accomplished by performing growth experiments using the Crystal Growth Furnace (CGF) manifested to fly on various Spacelab missions.

Lehoczky, Sandor L.↗
NASA NTRS1999

Reducing and Inducing Convection in Ge-Si Melts with Static Magnetic Field

Results of a study of the effectiveness of using static magnetic fields to reduce convection in Ge-Si melts will be presented. Lenz's law causes a retardation of convection when a static magnetic field is applied to an electrically conducting liquid. However, during the solidification of a solid-solution system such as Ge-Si, the interface is neither isothermal nor isoconcentrational. The variation of temperature and chemical composition along the interface causes thermoelectric currents to be generated within the solidifying material (and the container if it is electrically conductive). These currents, in the presence of a magnetic field, can cause movement (stirring, convection) in the melt which can exceed convection induced by normal thermosolutal mechanisms. Crystals have been grown by both the Bridgman and floating-zone methods. Clear evidence for the existence of this thermoelectromagnetic convection, especially in the case of Si floating-zone growth, will be presented.

Szofran, Frank R.↗