The free energy of formation of tantalum silicides using solid oxide electrolytes.
Free energies of formation determined for tantalum silicides from EMF measurements on cells with solid thoria-yttria electrolytes
Kolodney, M.↗
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Exploratory study of silicide, aluminide, and boride coatings for nitridation/oxidation protection of chromium alloys
Silicide, aluminide and boride coatings transition temperature holdability, considering nitridation/ oxidation protection for Cr alloys
Klopp, W. D.↗
Oxidation/vaporization of silicide coated columbium base alloys
Mass spectrometric and target collection experiments were made at 1600 K to elucidate the mode of oxidative vaporization of two columbium alloys, fused-slurry-coated with a complex silicide former (Si-20Cr-Fe). At oxygen pressures up to 0.0005 torr the major vapor component detected by mass spectrometry for oxidized samples was gaseous silicon monoxide. Analysis of condensates collected at oxygen pressures of 0.1, 1.0 and 10 torr revealed that chromium-, silicon-, iron- and tungsten- containing species were the major products of vaporization. Equilibrium thermochemical diagrams were constructed for the metal-oxygen system corresponding to each constituent metal in both the coating and base alloy. The major vaporizing species are expected to be the gaseous oxides of chromium, silicon, iron and tungsten. Plots of vapor phase composition and maximum vaporization rate versus oxygen pressure were calculated for each coating constituent. The major contribution to weight loss by vaporization at oxygen pressures above 1 torr was shown to be the chromium-containing species.
Kohl, F. J.↗
Practical field repair of fused slurry silicide coating for space shuttle t.p.s.
Study of short-time high-temperature diffusion treatments as part of a program of development of methods of reapplying fused slurry silicide coating in the field. The metallographic structure and oxidation behavior of R512E applied to Cb-752 coated under simulated field repair conditions was determined. Oxidation testing in reduced pressure environment has shown that performance equivalent to furnace-processed specimens can be obtained in a two-minute diffusion at 2700 F.
Reznik, B. D.↗
Fusion silicide coatings for tantalum alloys.
Calculation of the performance of fusion silicide coatings under simulated atmospheric reentry conditions to a maximum temperature of 1810 K (2800 F). Both recently developed and commercially available coatings are included. Data are presented on oxidation rate with and without intentional defecting, the influence of the coatings on the ductile-brittle bend transition temperature, and the mechanical properties. Coatings appear capable of affording protection for at least 100 simulated cycles to 2600 F and 63 cycles to 2800 F.
Warnock, R. V.↗
Oxidation at through-hole defects in fused slurry silicide coated columbium alloys FS-85 and Cb-752
Metal recession and interstitial contamination at 0.08-centimeter-diameter through-hole intentional defects in fused slurry silicide coated FS-85 and Cb-752 columbium alloys were studied to determine the tolerance of these materials to coating defects. Five external pressure reentry simulation exposures to 1320 C and 4.7 x 1,000 N/sq m (maximum pressure) resulted in a consumed metal zone having about twice the initial defect diameter for both alloys with an interstitial contamination zone extending about three to four initial defect diameters. Self-healing occurred in the 1.33 x 10 N/sq m, 1320 C exposures and to a lesser extent in internal pressure reentry cycles to 1320 C and 1.33 x 100 N/sq m (maximum pressure).
Levine, S. R.↗
Modified fused silicide coatings for tantalum (Ta-10W) reentry heat shields
Results are presented of a program of research to develop a reliable, high performance, fused slurry silicide coating for the Ta-10W alloy. The effort was directed toward developing new and improved formulations for use at 2600 to 2800 F (1700 to 1811 K) in an atmospheric reentry thermal protection system with a 100-mission capability. Based on a thorough characterization of isothermal and cyclic oxidation behavior, bend transition temperatures, room- and elevated-temperature tensile properties, and creep behavior, a 2.5 Mn-33Ti-64.5Si coating (designated MTS) provides excellent protection for the Ta-10W alloy in simulated reentry environments. An extensive analysis of the oxidation behavior and characteristics of the MTS coating in terms of fundamental mechanisms also is presented.
Packer, C. M.↗
Fused slurry silicide coatings for columbium alloys reentry heat shields. Volume 1: Evaluation analysis
The R-512E (Si-20Cr-20Fe) fused slurry silicide coating process was optimized to coat full size (20in x 20in) single face rib and corrugation stiffened panels fabricated from FS-85 columbium alloy for 100 mission space shuttle heat shield applications. Structural life under simulated space shuttle lift-off stresses and reentry conditions demonstrated reuse capability well beyond 100 flights for R-512E coated FS-85 columbium heat shield panels. Demonstrated coating damage tolerance showed no immediate structural failure on exposure. The FS-85 columbium alloy was selected from five candidate alloys (Cb-752, C-129Y, WC-3015, B-66 and FS-85) based on the evaluation tests which have designed to determine: (1) change in material properties due to coating and reuse; (2) alloy tolerance to coating damage; (3) coating emittance characteristics under reuse conditions; and (4) new coating chemistries for improved coating life.
Fitzgerald, B.↗
Fused slurry silicide coatings for columbium alloy reentry heat shields. Volume 2: Experimental and coating process details
The experimental and coating process details are presented. The process specifications which were developed for the formulation and application of the R-512E fused slurry silicide coating using either an acrylic or nitrocellulose base slurry system is also discussed.
Fitzgerald, B.↗
Friction and wear of radiofrequency-sputtered borides, silicides, and carbides
The friction and wear properties of several refractory compound coatings were examined. These compounds were applied to 440 C bearing steel surfaces by radiofrequency (RF) sputtering. The refractory compounds were the titanium and molybdenum borides, the titanium and molybdenum silicides, and the titanium, molybdenum, and boron carbides. Friction testing was done with a pin-on-disk wear apparatus at loads from 0.1 to 5.0 newtons. Generally, the best wear properties were obtained when the coatings were bias sputtered onto 440 C disks that had been preoxidized. Adherence was improved because of the better bonding of the coatings to the iron oxide formed during preoxidation. As a class the carbides provided wear protection to the highest loads. Titanium boride coatings provided low friction and good wear properties to moderate loads.
Brainard, W. A.↗
An XPS study of the adherence of refractory carbide, silicide, and boride RF-sputtered wear-resistant coatings
Radio frequency sputtering was used to deposit refractory carbide, silicide, and boride coatings on 440-C steel substrates. Both sputter etched and pre-oxidized substrates were used and the films were deposited with and without a substrate bias. The composition of the coatings was determined as a function of depth by X-ray photoelectron spectroscopy combined with argon ion etching. Friction and wear tests were conducted to evaluate coating adherence. In the interfacial region there was evidence that bias may produce a graded interface for some compounds. Biasing, while generally improving bulk film stoichiometry, can adversely affect adherence by removing interfacial oxide layers. Oxides of all film constituents except carbon and iron were present in all cases but the iron oxide coverage was only complete on the preoxidized substrates. The film and iron oxides were mixed in the MoSi2 and Mo2C films but layered in the Mo2B5 films. In the case of mixed oxides, preoxidation enhanced film adherence. In the layered case it did not.
Brainard, W. A.↗
Ensuring the Consistency of Silicide Coatings
Diagram specifies optimum fusing time for given thicknesses of refractory metal-silicide coatings on columbium C-103 substrates. Adherence to indicated fusion times ensures consistent coatings and avoids underdiffusion and overdiffusion. Accuracy of diagram has been confirmed by tests.
Ramani, V.↗
Optical response at 10.6 microns in tungsten silicide Schottky barrier diodes
Optical response to radiation at a wavelength of 10.6 microns in tungsten silicide-silicon Schottky barrier diodes has been observed. Incident photons excite electrons by means of junction plasmon assisted inelastic electron tunneling. At 78 K, a peak in the second derivative of current versus junction bias voltage was observed at a voltage corresponding to the energy of photons having a wavelength of 10.6 microns. This peak increased with increasing incident laser power, saturating at the highest laser powers investigated.
Kumar, Sandeep↗
Narrow bandgap semiconducting silicides: Intrinsic infrared detectors on a silicon chip
Polycrystalline thin films of CrSi2, LaSi2, and ReSi2 were grown on silicon substrates. Normal incidence optical transmittance and reflectance measurements were made as a function of wavelength. It was demonstrated that LaSi2 is a metallic conductor, but that CrSi2 and ReSi2 are, in fact, narrow bandgap semiconductors. For CrSi2, the complex index of refraction was determined by computer analysis of the optical data. From the imaginary part, the optical absorption coefficient was determined as a function of photon energy. It was shown that CrSi2 possesses an indirect forbidden energy gap of slightly less than 0.31 eV, and yet it is a very strong absorber of light above the absorption edge. On the other hand, the ReSi2 films exhibit an absorption edge in the vicinity of 0.2 eV. Measurements of the thermal activation energy of resistivity for ReSi2 indicate a bandgap of 0.18 eV. It is concluded that the semiconducting silicides merit further investigation for development as new silicon-compatible infrared detector materials.
Mahan, John E.↗
Characteristics of a promising new thermoelectric material - Ruthenium silicide
A preliminary study on arc-melted samples has indicated that ruthenium silicide has the potential to obtain figure-of-merit values four times higher than that of conventional silicon-germanium material. In order to realize the high figure-of-merit values, high-quality crystal from the melt is needed. A Bridgman-like method has been employed and has realized much better crystals than arc-melted ones.
Ohta, Toshitaka↗
Narrow bandgap semiconducting silicides: Intrinsic infrared detectors on a silicon chip
Work done during the final report period is presented. The main technical objective was to achieve epitaxial growth on silicon of two semiconducting silicides, ReSi2 and CrSi2. ReSi2 thin films were grown on (001) silicon wafers by vacuum evaporation of rhenium onto hot substrates in ultrahigh vacuum. The preferred epitaxial relationship was found to be ReSi2(100)/Si(001) with ReSi2(010) parallel to Si(110). The lattice matching consists of a common unit mesh of 120 A(sup 2) area, and a mismatch of 1.8 percent. Transmission electron microscopy revealed the existence of rotation twins corresponding to two distinct but equivalent azimuthal orientations of the common unit mesh. MeV He(+) backscattering spectrometry revealed a minimum channeling yield of 2 percent for an approximately 1,500 A thick film grown at 650 C. Although the lateral dimension of the twins is on the order of 100 A, there is a very high degree of alignment between the ReSi2(100) and the Si(001) planes. Highly oriented films of CrSi2 were grown on (111) silicon substrates, with the matching crystallographic faces being CrSi2(001)/Si(111). The reflection high-energy electron diffraction (RHEED) patterns of the films consist of sharp streaks, symmetrically arranged. The predominant azimuthal orientation of the films was determined to be CrSi2(210) parallel to Si(110). This highly desirable heteroepitaxial relationship has been obtained previously by others; it may be described with a common unit mesh of 51 A(sup 2) and mismatch of 0.3 percent. RHEED also revealed the presence of limited film regions of a competing azimuthal orientation, CrSi2(110) parallel to Si(110). A channeling effect for MeV He(+) ions was not found for this material. Potential commercial applications of this research may be found in silicon-integrated infrared detector arrays. Optical characterizations showed that semiconducting ReSi2 is a strong absorber of infrared radiation, with the adsorption constant increasing above 2 x 10(exp 4) cm(sup -1) for photon energies above 0.2 eV. CrSi2 is of potential utility for detection at photon energies above approximately 0.3 eV.
Mahan, John E.↗
A promising new thermoelectric material - Ruthenium silicide
Experimental and theoretical efforts directed toward increasing thermoelectric figure of merit values by a factor of 2 or 3 have been encouraging in several respects. An accurate and detailed theoretical model developed for n-type silicon-germanium (SiGe) indicates that ZT values several times higher than currently available are expected under certain conditions. These new, high ZT materials are expected to be significantly different from SiGe, but not unreasonably so. Several promising candidate materials have been identified which may meet the conditions required by theory. One such candidate, ruthenium silicide, currently under development at JPL, has been estimated to have the potential to exhibit figure of merit values 4 times higher than conventional SiGe materials. Recent results are summarized.
Vining, Cronin B.↗
Progress in doping of ruthenium silicide (Ru2Si3)
Ruthenium silicide is currently under development as a promising thermoelectric material suitable for space power applications. Key to realizing the potentially high figure of merit values of this material is the development of appropriate doping techniques. In this study, manganese and iridium have been identified as useful p- and n-type dopants, respectively. Resistivity values have been reduced by more than 3 orders of magnitude. Anomalous Hall effect results, however, complicate interpretation of some of the results and further effort is required to achieve optimum doping levels.
Vining, C. B.↗