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Continuous process has economic and quality advantages over batch processes. Expected to produce high-quality microballoons at relatively low cost. Continuous hollow-jet process produces microballoons of refractory metal. Microballoon products made by continuous process includes inertial-confinement fusion targets, thermal insulators, lightweight composites, impact absorbers, and containers for hazardous materials.
Tendency toward gas porosity exploited. Falling through drop tube, fine drops of molten metal lose heat to surroundings, forming hard shells around precipitated gas. Second heating/cooling cycle in drop tube of lower pressure lets gas expand. Process produces smaller shells in greater variety of materials than possible with such current processes as based on hollow-jet instability, dry-chemical blowing or fluid-droplet drying. Shell aspect ratio (ratio of radius to wall thickness) controllable. New process makes shells having diameters smaller than 100 micrometer. There are several candidate shell materials including refractory metals.
Space power requirements for future NASA and other U.S. missions will range from a few kilowatts to megawatts of electricity. Maximum efficiency is a key goal of any power system in order to minimize weight and size so that the space shuttle may be used a minimum number of times to put the power supply into orbit. Nuclear power has been identified as the primary source to meet these high levels of electrical demand. One way to achieve maximum efficiency is to operate the power supply, energy conversion system, and related components at relatively high temperatures. NASA Lewis Research Center has undertaken a research program on advanced technology of refractory metal alloys and composites that will provide baseline information for space power systems in the 1900's and the 21st century. Basic research on the tensile and creep properties of fibers, matrices, and composites is discussed.
The oxygen and magnesium isotopic compositions of five individual particles that were collected from the stratosphere and that bear refractory minerals were measured by secondary ion mass spectrometry. Four of the particles exhibit excesses of oxygen-16 similar to those observed in anhydrous mineral phases of carbonaceous chondrites and thus are extraterrestrial. The oxygen and magnesium isotopic abundances of one corundum-rich particle are consistent with a terrestial origin. Magnesium in the four extraterrestrial particles is isotopically normal. It is unlikely that these particles are derived from carbonaceous chondrites and thus such particles probably represent a new type of collected extraterrestrial material.
Thermoelectric energy conversion utilizing nuclear heat sources has been employed for several decades to generate power for deep space probes. In the past, lead telluride and, more recently, silicon-germanium alloys have been the prime choices as thermoelectric materials for this application. Currently, a number of refractory semiconductors are under investigation at the Jet Propulsion Laboratory in order to produce power sources of higher conversion efficiency and, thus, lower mass per unit of power output. Included among these materials are improved Si-Ge alloys, rare earth compounds and boron-rich borides. The criteria used to select thermoelectric materials, in general, and the above materials, in particular, will be discussed. The current state of the art and the accomplishments to date in thermoelectric materials research will be reviewed.
Experimental studies indicate that opaque assemblages rich in refractory siderophile elements were formed within host calcium- and aluminum-rich inclusions (CAIs) by exsolution, oxidation and sulphidization of homogeneous alloys, rather than by aggregation of materials in the solar nebula before the formation of CAIs. These opaque assemblages are thus not the oldest known solid materials, as was once thought, and they do not constrain processes in the early solar nebula before CAI formation. Instead, the assemblages record the changing oxygen fugacity experienced by CAIs during slow cooling in nebular and/or planetary environments.
Histories of refractory interstellar dust particles (IDPs) are calculated. The profile of a particle population is assembled from a large number of stochastic, or Monte Carlo, histories of single particles; the probabilities for each of the events that may befall a given particle are specified, and the particle's history is unfolded by a sequence of random numbers. The assumptions that are made and the techniques of the calculation are described together with the results obtained. Several technical demonstrations are presented.
The refractory inclusions embedded in the matrix of many carbonaceous and some ordinary or enstatite chondrites exhibit mineralogical and bulk composition characteristics which correlate with the first, or highest-temperature, condensation products that have been predicted to form from a hot, but cooling, solar nebula. These inclusions' isotopic compositions indicate presolar nucleosynthetic processes that have contributed to the production of the elements from which the solar system was formed; subsequently, the inclusions experienced melting, recrystallization, and alteration histories that have obscured the formation processes.
This paper reports preliminary measurements of the oxygen isotopic fractionation that occurs during the condensation of refractory metal oxide smokes. Fractionation occurred at temperatures in excess of 500 K during and/or subsequent to reaction of SiH4, Fe(CO)5, Al(CH3)3, and O2 in a H2 carrier gas. Observed isotopic fractionation was as high as -15 per mil/amu. The magnitude of the isotopic fractionation suggests that the process is kinetically controlled since the effect is greatly in excess of that expected for equilibrium isotopic exchange.
The results of a number of experiments are reported in which SiH4-Fe(CO)5-H2O ice mixtures were irradiated by 1 MeV protons at 15 K and then warmed to room temperature in approximately 50 K steps. The properties of a sample were monitored by observing its infrared absorption spectrum as a function of its processing history. In each experiment in which ice samples containing SiH4 were irradiated, a refractory amorphous silicate residue remained after warming to room temperature. In addition to the usual broad silicate features at 10 and 20 microns, features due to water or hydroxyl at 3 and 6.2 microns, and a feature due to CO at 5 microns, a surprisingly stable infrared feature at 4.6 microns, attributed to the SiH stretching fundamental, was observed.
A sputtering and recycling Monte Carlo model, developed by Liffman and Clayton (1988) is used to calculate the distribution of existence times of the matter in interstellar dust composed of refractory metals. The mean age of each dust particle is defined not as the time it has existed but rather as the mass-weighted existence times of its parts at t = 6 Gyr of the modeled solar system formation. It is shown that Galactic evolution generates a mean correlation, applying to large numbers of particles binned according to size rather than according to individual particles, whose mean ages fluctuate statistically. The cosmochemical consequence is that if interstellar particles can be dynamically sorted into separate size populations during the aggregation history of solar system bodies, the collections of larger grains will constitute matter that is chemically older than collections of smaller grains. The macroscopic age difference generates isotopic anomalies by virtue of the time dependence of the secondary/primary nucleosynthesis yields. Results are compared with three different prescriptions for the sputtering of interstellar dust.
Ca-Al-rich inclusions (CAIs) in refractory meteorites are shown to have been subject to partial melting during a suitably high gas density/small scale height regime arising during gasdynamic deceleration in a temporary atmosphere around an accreting parent body. The presence of dust in such an atmosphere would have increased the pressure gradient with height, lowering the boiloff rate, and permitting dust particles to become trapped in the partially melted material. CAIs may therefore be studied as probes of a primitive atmosphere.
Concepts for future space power systems include nuclear and focused solar heat sources coupled to static and dynamic power-conversion devices; such systems must be designed for service lives as long as 30 years, despite service temperatures of the order of 1600 K. Materials are a critical technology-development factor in such aspects of these systems as reactor fuel containment, environmental protection, power management, and thermal management. Attention is given to the prospective performance of such refractory metals as Nb, W, and Mo alloys, W fiber-reinforced Nb-matrix composites, and HfC precipitate-strengthened W-Re alloys.
Studies of the properties of refractory metal oxide smokes condensed from a gas containing various combinations of SiH4, Fe(CO)5, Al(CH3)3, TiCl4, O2 and N2O in a hydrogen carrier stream at 500 K greater than T greater than 1500 K were performed. Ultraviolet, visible and infrared spectra of pure, amorphous SiO(x), FeO(x), AlO(x) and TiO(x) smokes are discussed, as well as the spectra of various co-condensed amorphous oxides, such as FE(x)SiO(y) or Fe(x)AlO(y). Preliminary studies of the changes induced in the infrared spectra of iron-containing oxide smokes by vacuum thermal annealing suggest that such materials become increasingly opaque in the near infrared with increased processing: hydration may have the opposite effect. More work on the processing of these materials is required to confirm such a trend: this work is currently in progress. Preliminary studies of the ultraviolet spectra of amorphous Si2O3 and MgSiO(x) smokes revealed no interesting features in the region from 200 to 300 nm. Studies of the ultraviolet spectra of both amorphous, hydrated and annealed SiO(x), TiO(x), AlO(x) and FeO(x) smokes are currently in progress. Finally, data on the oxygen isotopic composition of the smokes produced in the experiments are presented, which indicate that the oxygen becomes isotopically fractionated during grain condensation. Oxygen in the grains is as much as 3 percent per amu lighter than the oxygen in the original gas stream. The authors are currently conducting experiments to understand the mechanism by which fractionation occurs.
Available creep data for the refractory-metal alloys C-103 (Nb/10 percent Hf/1 percent Ti/0.7 percent Zr), ASTAR-811C (Ta/8 percent W/1 percent Re/0.7 percent Hf/0.025 percent C), W-5Re (W/5 percent Re), and W-25Re (W/25 percent Re) were correlated by the Orr-Sherby-Dorn method and extrapolated to 1 percent creep over 10 years. Useful life was specified to be 2 standard estimates of error below the mean surface through the data. Over the temperature range of 1200 to 1800 K, ASTAR-811C was found to be the strongest of these alloys. In particular, ASTAR-811C was found to have at 1800 K the same creep strength as W-25Re at 1420 K. The difference between these results and those of Horak and Booker likely devolves from the comparative lack of long-time data on tungsten alloys.
Atomic oxygen in LEO may have undesirable effects on exposed refractory materials, such as are proposed for nuclear reactors in orbit, high temperature radiators, solar dynamic collectors, etc. Time-resolved measurement of the volatile efflux from such materials at high temperatures is being done in an ultrahigh vacuum atomic oxygen ion beam facility. Results of measurements of the efflux of volatile oxides of molybdenum and niobium-1 percent zirconium at temperatures as high as 1550 K are presented, along with a discussion of the roles of adsorption, desorption, and diffusion in atomic oxygen reactions on surfaces at high temperatures. The dependence of reaction rates for certain materials on the energy of the incident atomic oxygen beam will be emphasized.
The discovery is reported of opaque assemblages in the Leoville carbonaceous chondrite with both clear textural and chemical evidence of a major role for resolution and equilibration at relatively low temperatures in the formation of refractory siderophile element-rich assemblages. The observed phase compositions are used to bracket a previously inferred phase boundary in the Fe-Ni-Ru system. The first meteoritic occurrence of goldmanite is also reported.
The objective of this investigation is to develop a technique with which refractory metal carbide samples can be exposed to hydrogen containing gases at high temperatures, and to use various microstructural and analytical techniques to determine the chemical and rate processes involved in hydrogen degradation in these materials. Five types of carbides were examined including WC, NbC, HfC, ZrC, and TaC. The ceramics were purchased and were all monolithic in nature. The temperature range investigated was from 850 to 1600 C with a hydrogen pressure of one atmosphere. Control experiments, in vacuum, were also conducted for comparison so that the net effects due to hydrogen could be isolated. The samples were analyzed prior to and after exposure. Gas samples were collected in selected experiments and analyzed using gas chromography. Characterization of the resulting microstructure after exposure to hydrogen was conducted using optical microscopy, x-ray diffraction, scanning electron microscopy, and weight change. The ceramics were purchased and were all monolithic in nature. It was found that all samples lost weight after exposure, both in hydrogen and vacuum. Results from the microstructure analyses show that the degradation processes are different among the five types of ceramics involved. In addition, the apparent activation energy for the degradation process is a function of temperature even within the same material. This indicates that there are more than one mechanism involved in each material, and that the mechanisms are temperature dependent.