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At least 37 records · Page 2

Preparation of tantalum-based alloys by a unique CVD process

The paper describes a sequential pulsing technique for deposition of refractory alloys and evaluates the technique for the deposition of the tantalum-base alloys Ta-10W (Ta-10 st% W) and T-111 (Ta-8 wt% W-2 wt% Hf). The deposition cycle for Ta-10W was chosen as alternate injections of TaCl5 plus hydrogen and WCl6 plus hydrogen. The cycle for T-111 was chosen as injections of TaCl5 plus hydrogen interspersed with injections of WCl6 plus hydrogen. A temperature range of 900-1300 C was chosen for both alloys. The ability of the pulse process to blanket a uniformly heated section of substrate with a mixture of gases, whose composition varies not with position on the substrate but instead with time of residence in the reactor, allows metal of uniform thickness to be deposited. It is shown that Ta and W can be deposited at high temperature with the formation of a dense columnar grain structure, so that the feasibility of preparing uniformly thick deposits of these elements by a 'pulsing' modification of CVD is demonstrated. A similar attempt to deposit T-111 was unsuccessful due to the difficulty in reducing HfCl4.

Bryant, W. A.↗

Processing, physical metallurgy and creep of NiAl + Ta and NiAl + Nb alloys

Powder processed NiAl + Ta alloys containing 1, 2, and 4.5 at percent tantalum and NiAl + Nb alloys containing 1 and 2 at percent niobium were developed for improved creep properties. In addition, a cast alloy with 5 at percent tantalum was also studied. Hot extrusion parameters for processing alloys with 1 and 2 at percent of tantalum or niobium were designed. The NiAl + 4.5 at percent Ta alloy could be vacuum hot pressed successfully, even though it could not be extruded. All the phases in the multiphase alloys were identified and the phase transformations studied. The Ni2AlTa in NiAl + 4.5 at percent Ta alloy transforms into a liquid phase above 1700 K. Solutionizing and annealing below this temperature gives rise to a uniform distribution of fine second phase precipitates. Compressive creep properties were evaluated at 1300 K using constant load and constant velocity tests. In the higher strain rate region single phase NiAl + 1 at percent Ta and NiAl + 1 at percent Nb alloys exhibit a stress exponent of 5 characteristic of climb controlled dislocation creep. In slower strain rate regime diffusional creep becomes important. The two phase alloys containing 2 to 5 at percent Ta and 2 at percent Nb show considerable improvement over binary NiAl and single phase alloys. Loose dislocation networks and tangles stabilized by the precipitates were found in the as crept microstructure. The cast alloy which has larger grains and a distribution of fine precipitates shows the maximum improvement over binary NiAl.

Pathare, Viren M.↗

Generation of long time creep data on refractory alloys at elevated temperatures

Ultrahigh vacuum creep tests were performed on tungsten, molybdenum, and tantalum alloys to develop design creep data and to evaluate the influence of liquid lithium exposure on the creep resistance of a tantalum alloy. Test conditions were generally selected to provide 1% creep in 1000 to 10,000 hours, with the test temperatures ranging between 1600 and 2900 F (1144 K and 1866 K). One percent creep life data from a tantalum-base T-111 alloy (Ta-8%W-2%Hf) were analyzed using a station function method to provide an improved parametric representation of the T-111 data. In addition, the minimum creep rate data from an ASTAR 811C alloy (Ta-8%W-1%Re-0.7%Hf0.025%C) were analyzed to determine the stress and temperature dependence of creep rate. Results of this analysis indicated that the activation energy for creep decreased from about 150 Kcal/mole (5130 J/mole) above 2400 F (1589 K) to about 110 Kcal/mole (3760 J/mole) below 2000 F (1361 K). This temperature range corresponds to the range where the creep mechanism changes from grain boundary sliding to intragranular creep.

Sheffler, K. D.↗

Thermal fatigue behavior of T-111 and ASTAR 811C in ultrahigh vacuum

The thermal fatigue behavior of the tantalum alloys T-111 (Ta-8W-2Hf) and ASTAR 811C (Ta-8W-1Re-0.7Hf-0.025C) has been evaluated using completely reversed push-pull fatigue tests conducted in ultrahigh vacuum with independently programmed temperature and strain cycles. Test results showed that cycling of the test temperature simultaneously with the mechanical strain in most cases significantly reduced the cycles to failure of both alloys compared to isothermal testing. Notched specimens had reduced lives under isothermal conditions, but the presence of a notch or use of a 1-h holdtime provided only a small further decrease in life for the temperature cycled tests. Compressive stress at the maximum temperature produced longer lives than tensile stress. ASTAR 811C was more fatigue resistant than T-111 isothermally and did not have as great a decrease in life with thermal cycling. Results are analyzed by partition of plastic strains into creep and creep-independent components and considering where each component was active in the hysteresis cycle.

Sheffler, K. D.↗

Effect of Reverse Bias Stress on Leakage Currents and Breakdown Voltages of Solid Tantalum Capacitors

The majority of solid tantalum capacitors are produced by high-temperature sintering of a fine tantalum powder around a tantalum wire followed by electrolytic anodization that forms a thin amorphous Ta2O5 dielectric layer and pyrolysis of manganese nitrite on the oxide to create a conductive manganese dioxide electrode. A contact to tantalum wire is used as anode terminal and to the manganese layer as a cathode terminal of the device. This process results in formation of an asymmetric Ta -- Ta2O5 -- MnO2 capacitor that has different characteristics at forward (positive bias applied to tantalum) and reverse (positive bias applied to manganese cathode) voltages. Reverse bias currents might be several orders of magnitude larger than forward leakage currents so I-V characteristics of tantalum capacitors resemble characteristics of semiconductor rectifiers. Asymmetric I-V characteristics of Ta -- anodic Ta2O5 systems have been observed at different top electrode materials including metals, electrolytes, conductive polymers, and manganese oxide thus indicating that this phenomenon is likely related to the specifics of the Ta -- Ta2O5 interface. There have been multiple attempts to explain rectifying characteristics of capacitors employing anodic tantalum pentoxide dielectrics. A brief review of works related to reverse bias (RB) behavior of tantalum capacitors shows that the mechanism of conduction in Ta -- Ta2O5 systems is still not clear and more testing and analysis is necessary to understand the processes involved. If tantalum capacitors behave just as rectifiers, then the assessment of the safe reverse bias operating conditions would be a relatively simple task. Unfortunately, these parts can degrade with time under reverse bias significantly, and this further complicates analysis of the I-V characteristics and establishing safe operating areas of the parts. On other hand, time dependence of reverse currents might provide additional information for investigation of the processes under reverse bias conditions. In practice, there were instances when, due to unforeseen events, the system operated at conditions when capacitors experience periodically a relatively small reverse bias for some time followed by normal, forward bias conditions. In such a case an assessment should be made on the degree to which these capacitors are degraded by application of low-voltage reverse bias, and whether this degradation can be reversed by normal operating conditions. In this study, reverse currents in different types of tantalum capacitors were monitored at different reverse voltages below 15%VR and temperatures in the range from room to 145 C for up to 150 hours to get better understanding of the degradation process and determine conditions favorable to the unstable mode of operation. The reversibility of RB degradation has been evaluated after operation of the capacitors at forward bias conditions. The effect of reverse bias stress (RBS) on reliability at normal operating conditions was evaluated using highly accelerated life testing at voltages of 1.5VR and 2 VR and by analysis of changes in distributions of breakdown voltages. Possible mechanisms of RB degradation are discussed.

Teverovsky, Alexander A.↗

Effects of Tantalum on the Temporal Evolution of a Model Ni-Al-Cr Superalloy During Phase Decomposition

The effects of a 2.0 at.% addition of Ta to a model Ni-10.0Al-8.5Cr (at.%) superalloy aged at 1073 K are assessed using scanning electron microscopy and atom-probe tomography. The gamma'(Ll2)-precipitate morphology that develops as a result of gamma-(fcc)matrix phase decomposition is found to evolve from a bimodal distribution of spheroidal precipitates, to {001}-faceted cuboids and parallelepipeds aligned along the elastically soft {001}-type directions. The phase compositions and the widths of the gamma'-precipitate/gamma-matrix heterophase interfaces evolve temporally as the Ni-Al-Cr-Ta alloy undergoes quasi-stationary state coarsening after 1 h of aging. Tantalum is observed to partition preferentially to the gamma'-precipitate phase, and suppresses the mobility of Ni in the gamma-matrix sufficiently to cause an accumulation of Ni on the gamma-matrix side of the gamma'/gamma interface. Additionally, computational modeling, employing Thermo-Calc, Dictra and PrecipiCalc, is employed to elucidate the kinetic pathways that lead to phase decomposition in this concentrated Ni-Al-Cr-Ta alloy.

Booth, Morrison, Christopher↗

Reversed Tantalum Capacitor Problem: A Failure to Fail, a Case Study

Reverse Ta capacitors are not expected to last for any length of time much less the over 74000 hours that they have been flying on Express (i.e. ExPRESS (Expedite the Processing of Experiments to the Space Station) Logistics Carrier (ELC) on the International Space Station. The report looks at the effects of moisture and temperature have on the capacitors. The removal of moisture has a far greater role in the survival of the capacitors than one would expect. Over 10000 hours of testing will be reviewed.

Shue, Jack↗

Effects of alloy composition in alleviating embrittlement problems associated with the tantalum alloy T-111

The causes of aging embrittlement in T-111 (Ta-8W-2Hf) and the effects of alloy modification were investigated. Results showed that T-111 contains a critical combination of tungsten and hafnium that leads to loss of ductility at -196 C after aging near 1040 C. This appears to occur because tungsten enhances hafnium segregation to grain boundaries and this also leads to increased susceptibility to hydrogen embrittlement. Aging embrittlement was not observed in tantalum alloys with reduced tungsten or hafnium contents; however, most of the alloys studied have lower strengths than T-111 and exhibit susceptibility to hydrogen embrittlement.

Stephens, J. R.↗

CALPHAD Models to Guide Refractory Alloys Additive Manufacturing: In-Situ Compounds Formation, Nanoparticles, and Impurities Considerations

This technical memorandum (TM) seeks to model and discuss aspects of nanoparticle and micrometer-scale particle or ‘microparticle’ inclusions in refractory metal alloy manufacturing, via a currently used additive manufacturing (AM) method that results in equivalent wt.% addition of dissolved elements in the melt pool composition and subsequent formation of nanometer-scale MC and MO inclusions. Additionally, the authors begin to consider the effects of oxygen (O), a ubiquitous impurity, in AM; and seek to understand a combined optimization of alloying, nano- and micro strengthening and refinement, elemental additions, and even in-situ compounds and alloys species formation. To gain insights, this TM focuses on a pair of refractory alloys currently of interest to NASA: tungsten-rhenium-tantalum carbide (with O impurities) (W-Re-TaC(-O)) and tungsten-rhenium-tantalum-carbon (with O impurities) (W-Re-Ta-C(-O)), which are processed via powder bed fusion (PBF)-SLM.

ICME integrated computational materials engineerin↗

Effects of alloy composition in alleviating embrittlement problems associated with the tantalum alloy T-111

The causes of aging embrittlement in T-111 (Ta-8W-2Hf) and the effect of alloy modification were investigated. Results show that T-111 possesses a critical combination of tungsten and hafnium that leads to loss in ductility at -196 C after aging near 1040 C. It was found that this occurs because tungsten enhances hafnium segregation to grain boundaries, which also leads to increased susceptibility to hydrogen embrittlement. Aging embrittlement was not observed in tantalum alloys with reduced tungsten or hafnium contents; most of the alloys studied have lower strengths than T-111 and exhibit susceptibility to hydrogen embrittlement.

Stephens, J. R.↗