Graphite-metal Composites Quarterly Report No. 2
Graphite effect on molybdenum-carbide composite properties and tungsten, vanadium, hafnium, tantalum, niobium, and zirconium metal systems
CARBON↗
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High Temperature Characteristics of Pt/TaSi2/Pt/W and Pt/Ti/W Diffusion Barrier Systems for Ohmic Contacts to 4H-SiC
The degradation of ohmic contacts to 4H-SiC pressure sensors over time at high temperature is primarily due to two failure mechanisms: migrating bond pad Au and atmospheric O toward the ohmic contact SiC interface and the inter-metallic mixing between diffusion barrier systems (DBS) and the underlying ohmic contact metallization. We investigated the effectiveness of Pt/TaSi2/Pt/W (DBS-A) and Pt/Ti/W (DBS-B) in preventing Au and O diffusion through the underlying binary Ti/W or alloyed W50:Ni50 ohmic contacts to 4H-SiC and the DBS ohmic contact intermixing at temperature up to 700 C.
Platinum↗
Solid solution and carbide strengthened arc melted tungsten alloys.
Solid solution and carbide strengthened arc melted alloys of hafnium with tungsten and ternary alloys of tantalum, columbium, rhenium and carbon
CARBIDE↗
Thin film process forms effective electrical contacts on semiconductor crystals
Process makes microscopic, low-resistance electrical contacts on hexagonal n-type silicon carbide crystals used for microelectronic devices. A vacuum deposition of aluminum is etched to expose the bare silicon carbide where the electrical contacts are made. Sputtering alternating layers of tantalum and gold forms the alloy film.
Formigoni, N. P.↗
Vapor pressure and evaporation rate of certain heat-resistant compounds in a vacuum at high temperatures
The vapor pressure and evaporation rate of borides of titanium, zirconium, and chrome; and of strontium and carbides of titanium, zirconium, and chrome, molybdenum silicide; and nitrides of titanium, niobium, and tantalum in a vacuum were studied. It is concluded that all subject compounds evaporate by molecular structures except AlB sub 12' which dissociates, losing the aluminum.
Bolgar, A. S.↗
Preparation of refractory cermet structures for lithium compatibility testing
High-purity nitride and carbide cermets were synthesized for compatability testing in liquid lithium. A process was developed for the preparation of high-purity hafnium nitride powder, which was subsequently blended with tungsten powder or tantalum nitride and tungsten powders and fabricated into 3 in diameter billets by uniaxial hot pressing. Specimens were then cut from the billets for compatability testing. Similar processing techniques were applied to produce hafnium carbide and zirconium carbide cermets for use in the testing program. All billets produced were characterized with respect to chemistry, structure, density, and strength properties.
Heestand, R. L.↗
The effects of tantalum on the microstructure of two polycrystalline nickel-base superalloys - B-1900 + Hf and MAR-M247
The effect of changing the content of Ta on the gamma/gamma-prime carbide microstructure was investigated in two crystalline nickel-base superalloys: conventionally cast B-1900 + Hf, and both conventionally cast and directionally solidified MAR-M247. The changes occurring in the microstructure effects were similar in both alloys. The gamma-prime and carbide volume fractions increased linearly with Ta additions, while the gamma-prime phase compositions did not change. Bulk Ta additions increased the levels of Cr and Co (in addition to that of Ta) of the gamma phase, a result of the approximately constant partitioning ratios for these two elements. The addition of Ta led to a partial replacement of Hf in the MC carbides. In addition, Cr-rich M(23)C(6) carbides formed as a result of MC carbide decomposition during heat treatment.
Heckel, R. W.↗
Adhesion and friction of transition metals in contact with nonmetallic hard materials
Sliding friction experiments were conducted with the metals yttrium, titanium, tantalum, zirconium, vanadium, neodymium, iron, cobalt, nickel, tungsten, platinum, rhenium, ruthenium, and rhodium in sliding contact with single crystal diamond, silicon carbide, pyrolytic boron nitride, and ferrite. Auger electron spectroscopy analysis was conducted with the metals and nonmetals to determine the surface chemistry and the degree of surface cleanliness. The results of the investigation indicate the adhesion and friction of the transition metals in contact with diamond, silicon carbide, boron nitride, and ferrite are related to the relative chemical activity of the metals. The more chemically active the metal, the higher the coefficient of friction and the greater amount of transfer to the nonmetals.
Miyoshi, K.↗
Thermodynamic properties of interstitial elements in the refractory metals Semiannual report, 1 Dec. 1966 - 31 May 1967
Partial molar free energies, enthalpies, and entropies of carbon dissolved in solid molybdenum, tungsten, niobium, and tantalum
THERMODYNAMIC PROPERTY↗
Materials review for improved automotive gas turbine engine
The potential role of superalloys, refractory alloys, and ceramics in the hottest sections of engines operating with turbine inlet temperatures as high as 1370 C is examined. The convential superalloys, directionally solidified eutectics, oxide dispersion strenghened alloys, and tungsten fiber reinforced superalloys are reviewed and compared on the basis of maximum turbine blade temperature capability. Improved high temperature protective coatings and special fabrication techniques for these advanced alloys are discussed. Chromium, columbium, molybdenum, tantalum, and tungsten alloys are also reviewed. Molbdenum alloys are found to be the most suitable for mass produced turbine wheels. Various forms and fabrication processes for silicon nitride, silicon carbide, and SIALON's are investigated for use in highstress and medium stress high temperature environments.
Belleau, C.↗
Development of advanced high strength tantalum base alloys. Phase 3: Influence of metallurgical condition on the mechanical properties of ASTAR-811C sheet
Metallurgical condition was shown to have a significant effect on the creep properties of ASTAR-811C (Ta-8W-1Re-0.7Hf-0.025C) sheet. Cold worked material exhibited creep rates 30 times higher than solution annealed material and 10 times greater than for recrystallized material. Both grain size and the carbide morphology changes as the final annealing temperature was raised from 3000 F to 3600 F. However, the lowest creep rates were achieved for material which retained the high temperature form of the Ta2C precipitate. Samples with GTA weldments had essentially identical properties as recrystallized base metal. Cooling rates from 3600 F of 5, 50, and 800 F deg/min. had little effect on the 2000 and 2400 F creep behavior of ASTAR-811C.
Ammon, R. L.↗
Structures for hypersonic airbreathing tactical missiles
The studies to date were encouraging and indicated that materials were available or could be developed to satisfy scramjet requirements. Some of the more promising materials for the critical components were indicated. This information is summarized as follows : (1) radome - Slip cast fused silica is the current candidate, but others are being investigated. One shortcoming of slip cast fused silica is its susceptability to rain damage. (2) inlet leading edges - A refractory metal with a good oxidation protective coating will be required. Tantalum T222 with a Hafnia coating looks promising. (3) inlet ducts - An uninsulated refractory alloy will be required. Columbium F-85 was the best of those considered for the noncircular ducts. (4) external body - The external body temperatures are sufficiently low to permit the use of super alloys. (5) combustor and nozzle - The pyrolytic graphite/silicon carbide coating is very attractive for use in the combustor and nozzle areas.
Caywood, W. C.↗
Iridium Interfacial Stack - IrIS
Iridium Interfacial Stack (IrIS) is the sputter deposition of high-purity tantalum silicide (TaSi2-400 nm)/platinum (Pt-200 nm)/iridium (Ir-200 nm)/platinum (Pt-200 nm) in an ultra-high vacuum system followed by a 600 C anneal in nitrogen for 30 minutes. IrIS simultaneously acts as both a bond metal and a diffusion barrier. This bondable metallization that also acts as a diffusion barrier can prevent oxygen from air and gold from the wire-bond from infiltrating silicon carbide (SiC) monolithically integrated circuits (ICs) operating above 500 C in air for over 1,000 hours. This TaSi2/Pt/Ir/Pt metallization is easily bonded for electrical connection to off-chip circuitry and does not require extra anneals or masking steps. There are two ways that IrIS can be used in SiC ICs for applications above 500 C: it can be put directly on a SiC ohmic contact metal, such as Ti, or be used as a bond metal residing on top of an interconnect metal. For simplicity, only the use as a bond metal is discussed. The layer thickness ratio of TaSi2 to the first Pt layer deposited thereon should be 2:1. This will allow Si from the TaSi2 to react with the Pt to form Pt2Si during the 600 C anneal carried out after all layers have been deposited. The Ir layer does not readily form a silicide at 600 C, and thereby prevents the Si from migrating into the top-most Pt layer during future anneals and high-temperature IC operation. The second (i.e., top-most) deposited Pt layer needs to be about 200 nm to enable easy wire bonding. The thickness of 200 nm for Ir was chosen for initial experiments; further optimization of the Ir layer thickness may be possible via further experimentation. Ir itself is not easily wire-bonded because of its hardness and much higher melting point than Pt. Below the iridium layer, the TaSi2 and Pt react and form desired Pt2Si during the post-deposition anneal while above the iridium layer remains pure Pt as desired to facilitate easy and strong wire-bonding to the SiC chip circuitry.
Spry, David↗
Thermal stability of the nickel-base superalloy B-1900 + Hf with tantalum variations
The microstructure of the solutionized and aged nickel-base superalloy B-1900 + Hf was examined after additional aging at 982 C for 72, 250, and 1000 hours. Alloy compositions that were examined contained the normal 1.34 at. pct (4.3 wt pct) Ta as well as 0.67 at. pct and zero Ta levels. The gamma-prime phase agglomerated, became platelike in morphology, and decreased in volume fraction for all three alloys throughout the aging treatments. Changes which occurred in the gamma and gamma-prime phase compositions were nearly complete after 72 hours of aging while changes in the MC carbide composition continued throughout the aging. Blocky M6C carbides precipitated along the grain boundaries of all three alloys in the first 72 hours of aging. In addition, an acicular form of this Mo/Cr/Ni-rich carbide developed in the intragranular regions of the Ta-containing alloys.
Harmon, B. S.↗
Development of advanced high strength tantalum base alloys. Part 1: Screening investigation
Five experimental tantalum alloy compositions containing 13-18% W+Re+Hf solid solution solute additions with dispersed phase strengthening achieved by carbon or nitrogen additions were prepared as 1.4 inch diameter ingot processed to 3/8 inch diameter rod and evaluated. Elevated temperature tensile and creep strength increased monotonically with increasing solute content. Room temperature elongation decreased for 20% to less than 2% as the solute content was increased above 16%. Phase identification indicated that the precipitating phase in the carbide containing alloys was Ta2C.
Buckman, R. W., Jr.↗
Influence of creep damage on the low cycle thermal-mechanical fatigue behavior of two tantalum base alloys
Low cycle fatigue tests have been performed on the tantalum base alloys T-111 and ASTAR 811C with synchronized, independently programmed temperature and strain cycling. The thermal-mechanical cycles applied fell into three basic categories: these were isothermal cycling, in-phase thermal cycling, and out-of-phase thermal cycling. In-phase cycling was defined as tensile deformation associated with high temperature and compressive deformation with low temperature, while out-of-phase thermal cycling was defined as the reverse case. The in-phase thermal cycling had a pronounced detrimental influence on the fatigue life of both alloys, with the life reduction being greater in the solid solution strengthened T-111 alloy than in the carbide strengthened ASTAR 811C alloy. The out-of-phase tests also showed pronounced effects on the fatigue life of both alloys, although not as dramatic.
Sheffler, K. D.↗
Generation of long time creep data on refractory alloys at elevated temperatures
Creep tests were conducted on two tantalum alloys (ASTAR 811C and T-111 alloy), on a molybdenum alloy (TZM), and on CVD tungsten. The T-111 alloy 1% creep life data have been subjected to Manson's station function analysis, and the progress on this analysis is described. In another test program, the behavior of T-111 alloy with continuously varying temperatures and stresses has been studied. The results indicated that the previously described analysis predicts the observed creep behavior with reasonable accuracy. In addition to the T-111 test program, conventional 1% creep life data have been obtained for ASTAR 811C alloy. Previously observed effects of heat treatment on the creep strength of this material have been discussed and a model involving carbide strengthening primarily at the grain boundaries, rather than in a classical dispersion hardening mechanism, has been proposed to explain the observed results.
Sheffler, K. D.↗
Creep behavior of tantalum alloy T-222 at 1365 to 1700 K
High vacuum creep tests on the tantalum T-222 alloy at 0.42 to 0.52 T sub m show that the major portion of the creep curves, up to at least 1 percent strain, can be best described by an increasing creep rate, with strain varying linearly with time. Correlation and extrapolation of the creep curves on the basis of increasing creep rates results in more accurate engineering design data than would use of approximated linear rates. Based on increasing creep rates, the stress for 1 percent strain in 10,000 hours for T-222 is about four times greater than for the Ta-10W alloy. Increasing the grain size results in increased creep strength. Thermal aging prior to testing caused precipitation of the hexagonal close packed (Hf,Ta) sub 2 C, which initially increased creep strength. However, this dimetal carbide was converted during creep testing to face-centered cubic (Hf,Ta)C.
Titran, R. H.↗