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Thermomechanical and Thermochemical Behavior of a Hafnium-20 Percent Tantalum Alloy

An investigation was conducted to determine the thermomechanical and thermochemical behavior of a high temperature, oxidation resistant, hafnium-20 percent tantalum alloy. The elastic and shear moduli of this alloy were determined in air up to 1000 C and in vacuum up to 2000 C using a mechanical resonance technique. The internal friction of the alloy was measured up to temperatures greater than 1400 C. Room temperature stress-strain behavior of the oxidized and unoxidized alloy was established. The effect of annealing on the elastic and shear moduli of the extruded rod material was investigated. The martensitic-type phase transformation occurring in the alloy was studied using hot stage metallography and electron microscopy. Static oxidation tests were conducted on the alloy at temperatures from 1000 C to 1700 C with weight gain measurements made as a function of time and temperatures. Surface morphology studies were conducted on the oxide coatings formed at the different temperatures using scanning electron microscopy and X-ray diffraction techniques.

Howell, J. P.↗

Effects of low-pressure air on oxygen contamination and lithium corrosion of a tantalum alloy, T-111, at 980 and 1260 C

The effects were studied of low-pressure air on contamination and corrosion in the tantalum alloy T-111/lithium system at 980 and 1260 C. Capsules of T-111 containing lithium were exposed to six vacuum levels between 1 x 10 to the 8th power and 0.0003 torr by controlled air leakage into a vacuum system. Capsules exposed at 980 C and 0.0002 torr failed from intragranular oxidation. The remainder of the capsules completed the 96-hour tests. The depth of oxygen contamination was greater at 980 C than at 1260 C. Tests made at 0.0001 and 0.00001 torr levels caused large increases in the oxygen content of the T-111. Tests at 0.000001 torr or less produced no significant contamination. No lithium corrosion of the T-111 was observed under any of the conditions.

Gahn, R. F.↗

Development of Coatings for Tantalum Alloy Nozzle Vanes

A group of silicide coatings developed for the T222 tantalum-base alloy have afforded over 600 hours of protection at 1600 and 2400 F during cyclic exposure in air. These coatings were applied in two steps. A modifier alloy was applied by slurry techniques and was sintered in vacuum prior to siliciding by pack cementation in argon. Application of the modifier alloy by pack cementation was found to be much less effective. The addition of titanium and vanadium to molybdenum and tungsten yielded beneficial modifier alloys, whereas the addition of chromium showed no improvement. After siliciding, the 15Ti- 35W-15V-35Mo modifier alloy exhibited the best performance; one sample survived 1064 hours of oxidation at 2400 F. This same coating was the only coating to reproducibly provide 600 hours of protection at both 1600 and 2400 F; in the second and third of three experiments, involving oxidation of three to five specimens at each temperature in each experiment, no failures were observed in 600 hours of testing. The slurry coatings were also shown to protect the Cb752 and D43 columbium-base alloys.

PROTECTIVE COATING↗

Tantalum alloys resist creep deformation at elevated temperatures

Dispersion-strengthened tantalum-base alloys possess high strength and good resistance to creep deformation at elevated temperatures in high vacuum environments. They also have ease of fabrication, good weldability, and corrosion resistance to molten alkali metals.

Buckman, R. W., Jr.↗

Mechanical properties of low tantalum alloys

The mechanical property behavior of equiaxed cast B-1900 + Hf alloy as a function of tantalum content was studied. Tensile and stress rupture characterization was conducted on cast to size test bars containing tantalum at the 4.3% (standard level), 2.2% and 0% levels. Casting parameters were selected to duplicate conditions used to prepare test specimens for master metal heat qualification. The mechanical property results as well as results of microstructural/phase analysis of failed test bars are presented.

Kortovich, C. S.↗

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.↗

Tantalum alloy–based resonators for quantum information systems

Utilizing tantalum (Ta) in superconducting circuits has led to significant improvements, such as high qubit lifetime (T 1 ) and quality factors in both qubits and resonators, suggesting that material optimization plays an important role in the development of superconducting circuits. Thus we here explore superconducting gap engineering in Ta-based devices as a powerful strategy for expanding the range of suitable host materials. By alloying 20 atomic percent (at.%) hafnium into Ta thin films, we achieve a superconducting transition temperature (T c ) of 6.09 K as observed in direct current (DC) transport measurements, reflecting an increase in the superconducting gap. We systematically vary deposition conditions to control film orientation and transport properties of Ta-Hf alloy thin films. We then confirm the enhancement in T c via microwave measurements at millikelvin temperatures. We verify the ~40 increase in T c relative to bare Ta devices, while the loss contributions from two-level systems and quasi-particles remain unchanged in the low temperature regime. These findings emphasize the promise of material engineering in superconducting circuits and point to many potential material candidates for further exploration.

Ta-Hf alloy thin films↗

Development of a fused slurry silicide coating for the protection of tantalum alloys

Results are reported of a research program to develop a reliable high-performance, fused slurry silicide protective coating for a tantalum-10 tungsten alloy for use at 1427 to 1538 C at 0.1 to 10 torr air pressure under cyclic temperature conditions. A review of silicide coating performance under these conditions indicated that the primary wear-out mode is associated with widening of hairline fissures in the coating. Consideration has been given to modifying the oxidation products that form on the coating surface to provide a seal for these fissures and to minimize their widening. On the basis of an analysis of the phase relationships between silica and various other oxides, a coating having the slurry composition 2.5Mn-33Ti-64.5Si was developed that is effective in the pressure range from 1 to 10 torr.

Packer, C. M.↗

Effect of aging at 1040 C (1900 F) on the ductility and structure of a tantalum alloy, T-111

The post-aging embrittlement of T-111 (tantalum - 8-percent tungsten - 2-percent hafnium) following exposure for up to about 10,000 hours at 1040 C in either vacuum or liquid lithium was investigated for sheet and tubing samples. This thermal aging was shown to greatly increase the sensitivity of T-111 to hydrogen embrittlement during subsequent room temperature specimen processing or testing. The hydrogen embrittlement problem can be avoided by preventing exposure to the T-111 to moisture during post-aging processing or testing. Aging at 1040 C also resulted in formation of HfO2 particles at grain boundaries, which may contribute to the observed embrittlement.

Watson, G. K.↗

Thermal expansion method for lining tantalum alloy tubing with tungsten

A differential-thermal expansion method was developed to line T-111 (tantalum - 8 percent tungsten - 2 percent hafnium) tubing with a tungsten diffusion barrier as part of a fuel element fabrication study for a space power nuclear reactor concept. This method uses a steel mandrel, which has a larger thermal expansion than T-111, to force the tungsten against the inside of the T-111 tube. Variables investigated include lining temperature, initial assembly gas size, and tube length. Linear integrity increased with increasing lining temperature and decreasing gap size. The method should have more general applicability where cylinders must be lined with a thin layer of a second material.

Watson, G. K.↗

Dissolution kinetics of small amounts of oxygen in tantalum alloy T-111 and internal oxide displacement reactions during annealing

Oxygen was added to T-111 (Ta-8W-2Hf, wt. %) at 820 and 990 C at an oxygen pressure of about 0.0003 torr. The technique employed permitted predetermined and reproducible doping of T-111 up to 3.0 at. % oxygen. Based on the temperature dependence of the doping reaction, it is concluded that the initial rates of oxygen pickup are probably controlled by solution of oxygen into the T-111 lattice. Although hafnium oxides are more stable than those of tantalum or tungsten, analyses of extracted residues indicate that the latter oxides predominate in the as-doped specimens, presumably because of the higher concentrations of tantalum and tungsten in the alloy. However, high-temperature annealing promotes gettering of dissolved oxygen and of other oxides to form hafnium oxides. Small amounts of tantalum and tungsten oxides were still present after high-temperature annealing. Tungsten oxide (WO3) volatilizes slightly from the surface of T-111 at 990 C. The vaporization of WO3 has no apparent affect on the doping reaction.

Stecura, S.↗

Techniques for lithium removal from 1040 C aged tantalum alloy, T-111

The liquid ammonia and vacuum distillation techniques were found to be satisfactory for removing lithium from 1040 C aged T-111 (tantalum - 8-percent tungsten- 2-percent hafnium). Results of ductility tests and chemical analysis show that these two methods are adequate for removing lithium without embrittlement or contamination of the T-111. Moist air exposure of T-111 with traces of lithium on the surface produced mixed results. Some specimens were ductile; others were brittle. Brittle T-111 had an increased hydrogen content. Water removal of lithium from T-111 caused brittleness and an increased hydrogen concentration.

Gahn, R. F.↗

Microstructural stability of tantalum-alloyed ferritic-martensitic steel with neutron irradiation to 7.4 dpa at ~490 °C

Specimens of a reduced-activation ferritic-martensitic steel, called CNA1, were irradiated to 7.4 displacements per atom at ~490 °C in the High Flux Isotope Reactor. Vickers hardness and tensile properties revealed consistent softening that is attributed to some recovery during irradiation, with reduced laths and dislocation density. Detailed microstructural characterization by transmission electron microscopy and energy dispersive x-ray spectroscopy showed radiation-induced dislocation loops, few cavities, and slight dissolution of M 23 C 6 and MX precipitates. Partial amorphization was only observed in M 23 C 6 precipitated in matrix. Transmutation somewhat destabilized M 23 C 6 and MX, with a stronger effect on the later one by noticeable depletion of Ta with enriched W, which is consistent with the transmutation calculations. The microstructural evolution and associated strength changes were discussed with the assistance of computational thermodynamics.

36 MATERIALS SCIENCE↗

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.↗

Study of gas tungsten arc welding procedures for tantalum alloy T-111 (Ta-8 W-2Hf) plate

Methods of eliminating or reducing underbread cracking in multipass GTA welds in thick T-111 plate were studied. Single V butt welds prepared using experimental filler metal compositions and standard weld procedures resulted in only moderate success in reducing underbread cracking. Subsequent procedural changes incorporating manual welding, slower weld speeds, and three or fewer fill passes resulted in crack-free single V welds only when the filler metal was free of hafnium. The double V joint design with successive fill passes on opposite sides of the joint produced excellent welds. The quality of each weld was determined metallographically since the cracking, when present, was very slight and undetectable using standard NDT techniques. Tensile and bend tests were performed on selected weldments. The inherent filler metal strength and the joint geometry determined the strength of the weldment. Hardness and electron beam microprobe traverses were made on selected specimens with the result that significant filler metal-base metal dilution as well as hafnium segregation was detected. A tentative explanation of T-111 plate underbread cracking is presented based on the intrinsic effects of hafnium in the weldment.

Gold, R. E.↗