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The 105-m drop tube at NASA/Marshall Space Flight Center has been used in a series of undercooling experiments on pure metals. Ti, Zr, Nb, Mo, Rh, Hf, Ta, and Pt were undercooled 17-20 percent of the melting temperature in a containerless, microgravity environment. Ir and Ru were undercooled to 13 percent Tm. Sample sizes ranged from 175 to 880 mg.
Growth of crystals on the surface of a Zr-Ba-La fluoride glass was observed by optical and scanning electron microscopy. Small, dark crystal nucleated rapidly and grew to a size of about 10 microns; then they stopped growing, and wrinkled regions emerged, covering the entire crystal surface.
Carbon arc electrical discharges struck across the surfaces of metals such as Nb-1 percent Zr, alter the morphology to produce a high thermal emittance surface. Metal from the surface and carbon from the arc electrode vaporize during arcing, and then condense on the metal surface to produce a microscopically rough surface having a high thermal emittance. Quantitative spectral reflectance measurements from 0.33 to 15 microns were made on metal surfaces which were carbon arc treated in an inert gas environment. The resulting spectral reflectance data were then used to calculate thermal emittance as a function of temperature for various methods of arc treatment. The results of arc treatment on various metals are presented for both ac and dc arcs. Surface characterization data, including thermal emittance as a function of temperature, scanning electron microscopy, and atomic oxygen durability, are also presented. The ac arc texturing was found to increase the thermal emittance at 800 K from 0.05 to 0.70.
The objective was to document finite-scale compositional variations in cumulate rocks from the Stillwater Complex in Montana and to interpret these data in the context of planetary magma fractionation processes such as those operative during the formation of the Earth's Moon. This research problem involved collecting samples in the Stillwater Complex and analyzing them by electron microprobe, X-ray fluorescence (XRF), and instrumental neutron activation analysis (INAA). The electron microprobe is used to determine the compositions of cumulus and intercumulus phases in the rocks, the XRF is used to determine the bulk-rock major element and trace element (Y, Sr, Rb, Zr, Ni, and Cr) abundances, and the INAA lab. is used to determine the trace element (Sc, Co, Cr, Ni, Ta, Hf, U, Th, and the REE) abundances of mineral separates and bulk rocks.
The 100-meter drop tube at NASA Marshall Space Flight Center provides an excellent opportunity to study the effects of containerless, microgravity processing in metals and alloys. In a series of experiments high melting temperature pure metals were melted in an electron beam furnace and dropped in vacuum. Sample sizes ranged from 0.175 to 1.2 grams. Large undercoolings on the order of 18 percent of the melting temperature were observed in Ti, Zr, Nb, Mo, Rh, Ta, and Pt. Undercoolings of 5 to 18 percent T(m) were observed in Ru and Ir. These undercooling results are consistent, repeatable, and occur in a high percentage of experiments. The experimental technique will be presented as well as the resultant microstructures of undercooled drops. The data will be discussed with respect to nucleation theory.
This paper presents a systematic thermodynamic analysis of the effects of temperature and composition on olivine/melt and low-Ca pyroxene/melt partitioning. Experiments were conducted in several synthetic basalts with a wide range of Fe/Mg, determining partition coefficients for Eu, Ca, Mn, Fe, Ni, Sm, Cd, Y, Yb, Sc, Al, Zr, and Ti and modeling accurately the changes in free energy for trace element exchange between crystal and melt as functions of the trace element size and charge. On the basis of this model, partition coefficients for olivine/melt and low-Ca pyroxene/melt can be predicted for a wide range of elements over a variety of basaltic bulk compositions and temperatures. Moreover, variations in partition coeffeicients during crystallization or melting can be modeled on the basis of changes in temperature and major element chemistry.
The oxidation of Ni-Al intermetallic alloys in the beta-NiAl phase field and in the two phase beta-NiAl/gamma'-Ni3Al phase field has been studied between 1000 and 1400 C. The stoichiometric beta-NiAl alloy doped with Zr was superior to other alloy compositions under cyclic and isothermal oxidation. The isothermal growth rates did not increase monotonically as the alloy Al content was decreased. The characteristically ridged alpha-Al2O3 scale morphology, consisting of cells of thin, textured oxide with thick growth ridges at cell boundaries, forms on oxidized beta-NiAl alloys. The correlation of scale features with isothermal growth rates indicates a predominant grain boundary diffusion growth mechanism. The 1200 C cyclic oxidation resistance decreases near the lower end of the beta-NiAl phase field.
Electrocatalysts and supports for the positive electrode of moderate temperature single-unit rechargeable alkaline fuel cells are being investigated and developed. Candidate support materials were drawn from transition metal carbides, borides, nitrides and oxides which have high conductivity (greater than 1 ohm/cm). Candidate catalyst materials were selected largely from metal oxides of the form ABO sub x (where A = Pb, Cd, Mn, Ti, Zr, La, Sr, Na, and B = Pt, Pd, Ir, Ru, Ni (Co) which were investigated and/or developed for one function only, O2 reduction or O2 evolution. The electrical conductivity requirement for catalysts may be lower, especially if integrated with a higher conductivity support. All candidate materials of acceptable conductivity are subjected to corrosion testing. Materials that survive chemical testing are examined for electrochemical corrosion activity. For more stringent corrosion testing, and for further evaluation of electrocatalysts (which generally show significant O2 evolution at at 1.4 V), samples are held at 1.6 V or 0.6 V for about 100 hours. The surviving materials are then physically and chemically analyzed for signs of degradation. To evaluate the bifunctional oxygen activity of candidate catalysts, Teflon-bonded electrodes are fabricated and tested in a floating electrode configuration. Many of the experimental materials being studied have required development of a customized electrode fabrication procedure. In advanced development, the goal is to reduce the polarization to about 300 to 350 mV. Approximately six support materials and five catalyst materials were identified to date for further development. The test results will be described.
A series of Cu-based alloys containing 2 to 10 a/o Cr and 1 to 5 a/o Nb were produced by chill block melt spinning (CBMS). The melt spun ribbons were consolidated and hot rolled to sheet to produce a supersaturated Cu-Cr-Nb solid solution from which the high melting point intermetallic compound Cr2Nb could be precipitated to strengthen the Cu matrix. The results show that the materials possess electrical conductivities in excess of 90 percent that of pure Cu at 200 C and above. The strengths of the Cu-Cr-Nb alloys were much greater than Cu, Cu-0.6 Cr, NARloy-A, and NARloy-Z in the as-melt spun condition. The strengths of the consolidated materials were less than Cu-Cr and Cu-Cr-Zr below 500 C and 600 C respectively, but were significantly better above these temperatures. The strengths of the consolidated materials were greater than NARloy-Z, at all temperatures. The GLIDCOP possessed similar strength levels up to 750 C when the strength of the Cu-Cr-Nb alloys begins to degrade. The long term stability of the Cu-Cr-Nb alloys was measured by the microhardness of aged samples and the growth of precipitates. The microhardness measurements indicate that the alloys overage rapidly, but do not suffer much loss in strength between 10 and 100 hours which confirms the results of the electrical resistivity measurements taken during the aging of the alloys at 500 C. The loss in strength from peak strength levels is significant, but the strength remains exceptionally good. Transmission electron microscopy (TEM) of the as-melt spun samples revealed that Cr2Nb precipitates formed in the liquid Cu during the chill block melt spinning, indicating a very strong driving force for the formation of the precipitates. The TEM of the aged and consolidated materials indicates that the precipitates coarsen considerably, but remain in the submicron range.
The development of a noncontact temperature measurement device utilizing rotating analyzer ellipsometry is described. The technique circumvents the necessity of spectral emissivity estimation by direct measurement concomittant with radiance brightness. Using this approach, the optical properties of electromagnetically levitated liquid metals Cu, Ag, Au, Ni, Pd, Pt, and Zr were measured in situ at four wavelengths and up to 600 K superheat in the liquid. The data suggest an increase in the emissivity of the liquid compared with the incandescent solid. The data also show moderate temperature dependence of the spectral emissivity. A few measurements of the optical properties of undercooled liquid metals were also conducted. The data for both solids and liquids show excellent agreement with available values in the literature for the spectral emissivities as well as the optical constants.
The Advanced Composition Explorer (ACE) was recently selected as one of two new Explorer-class missions to be developed for launch during the mid-1990's. ACE will observe particles of solar, interplanetary, interstellar, and galactic origins, spanning the energy range from that of the solar wind (approx. 1 keV/nucleon) to galactic cosmic ray energies (several hundred MeV/nucleon). Definitive studies will be made of the abundance of nearly all isotopes from H to Zn (1 less than or = Z less than or = 30), with exploratory isotope studies extending to Zr (Z = 40). To accomplish this, the ACE payload includes six high-resolution spectrometers, each designed to provide the optimum charge, mass, or charge-state resolution in its particular energy range, and each having a geometry factor optimized for the expected flux levels, so as to provide a collecting power a factor of 10 to 1000 times greater than previous or planned experiments. The payload also includes several instruments of standard design that will monitor solar wind and magnetic field conditions and energetic H, He, and electron fluxes. The scientific objectives, instrumentation, spacecraft, and mission approach that were defined for ACE during the Phase-A study period are summarized.
The effect of a zirconium addition (0.05 at. pct) to a stoichiometric NiAl alloy on the brittle-to-ductile transition temperature (BDTT) of this alloy was investigated. Constant velocity tensile tests were conducted to fracture between 300 and 1100 K under initial strain rate 0.00014/sec, and the true stress and true strain values were determined from plots of load vs time after subtracting the elastic strain. The inelastic strain was measured under a traveling microscope. Microstructural characterization of as-extruded and fractured specimens was carried out by SEM and TEM. It was found that, while the addition of 0.05 at. pct Zr strengthened the NiAl alloy, it increased its BDTT; this shift in the BDTT could not be attributed either to variations in grain size or to impurity contents. Little or no room-temperature ductility was observed for either alloy.
The applicability of ion microprobe (IMP) for quantitative analysis of minor elements (Sr, Y, Zr, La, Sm, and Yb) in the major phases present in natural Ca-, Al-rich inclusions (CAIs) was investigated by comparing IMP results with those of an electron microprobe (EMP). Results on three trace-element-doped glasses indicated that it is not possible to obtain precise quantitative analysis by using IMP if there are large differences in SiO2 content between the standards used to derive the ion yields and the unknowns.
The present conference on the high-temperature oxidation behavior of aerospace structures-applicable intermetallic compounds discusses the influence of reactive-element additions on the oxidation of Ni3Al base alloys, the effect of Ni3Al oxidation below 850 C on fracture behavior, the oxidation of FeAl + Hf, Zr, and B, the synergistic effect of Al and Si on the oxidation resistance of Fe alloys, and pack cementation coatings of Cr-Al on Fe, Ni, and Co alloys. Also discussed are the formation of alumina on Nb- and Ti-base alloys, the oxidation behavior of titanium aluminide alloys, silicide coatings for refractory metals, the oxidation of chromium disilicide, and the oxidation behavior of nickel beryllides.
The oxidation of Ni-Al intermetallic alloys in the beta-NiAl phase field and in the two phase beta-NiAl/gamma'-Ni3Al phase field has been studied between 1000 and 1400 C. The stoichiometric beta-NiAl alloy doped with Zr was superior to other alloy compositions under cyclic and isothermal oxidation. The isothermal growth rates did not increase monotonically as the alloy Al content was decreased. The characteristically ridged alpha-Al203 scale morphology, consisting of cells of thin, textured oxide with thick growth ridges at cell boundaries, forms on oxidized beta-NiAl alloys. The correlation of scale features with isothermal growth rates indicates a predominant grain boundary diffusion growth mechanism. The 1200 C cyclic oxidation resistance decreases near the lower end of the beta-NiAl phase field.
Results are presented on recent studies of refractory-metal-alloy and refractory-metal-composite technologies for space power systems, with emphasis on work performed at the Lewis Research Center in support of the Ground Engineering System (GES) for the SP-100 reactor. Special attention is given to the mechanical properties of alloys with compositions Nb-1Zr and Nb-0.1Zr-0.1C (the PWC-11 alloy) and to advanced fiber-reinforced composites. The results to date indicate that, for the GES at a power level of about 100 kWe, the PWC-11 has attractive creep properties that will extend the capabilities of the SP-100 reactor compared to a similar system fabricated from Nb-1Zr. On the other hand, tungsten-reinforced Nb-1Zr composites were found to provide a ten-fold and four-fold creep strength over Nb-1Zr and PWC-11, respectively, at 1400 to 1500 K.
Tests were carried out to assess the impact of wind blown dust accumulation and abrasion on radiator surfaces on Mars. High emittance arc-textured copper and niobium-1 percent-zirconium samples were subjected to basaltic dust laden wind at Martian pressure (1000 Pa) at speeds varying from 19 to 97 m/s in the Martian Surface Wind Tunnel. The effect of accumulated dust was also observed by pre-dusting some of the samples before the test. Radiator degradation was determined by measuring the change in the emittance after dust was deposited and/or removed. The principle mode of degradation was abrasion. Arc textured Nb-1 percent-Zr proved to be more susceptible to degradation than Cu, and pre-dusting appeared to have lessened the abrasion.
Exposed and unexposed (shielded) portions of the surfaces of six different metal samples (Al, Cu, Ni, Ta, W, and Zr) that had been mounted on LDEF were studied by variable angle spectroscopic ellipsometry. The change in the optical constants of the metals caused by exposure to the space environment was measured. The measured optical constants reflect changes in the morphology and stoichiometry of a surface layer to a depth of this order of magnitude. For all the samples examined in this manner the exposed and unexposed portions exhibited dramatically different optical properties. In order to determine whether the observed changes were caused by the impact of oxygen atoms encountered in flight an experiment was set up in which samples identical to the original metal samples are exposed to a low-energy oxygen plasma in a microwave discharge chamber. Results of this experiment are reported, as well as an analysis of the observed data in terms of surface layers of different composition.