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At least 19 records
All sourcesNASA NTRSDOE OSTI
DOE OSTI2024

Observation of tantalum deposition and growth on TiB2 and ZrB2 from PISCES-RF deuterium and helium plasma exposures

Deuterium and helium plasma exposures on bulk TiB2 and ZrB2 samples were performed using the PISCES-RF linear plasma device. 40 and 90 eV deuterium ion plasma exposures were performed at 240 and 800 °C sample temperatures, and 80 eV helium ion plasma exposures were performed at 800 °C sample temperatures. Following plasma exposures, it was discovered that two plasma conditions (90 eV deuterium and 80 eV helium at 800 °C) resulted in thick (>200 nm) tantalum-rich (>10 at%) surface features on the targets, presumably from tantalum sourced from a tantalum adapter mask or cap used as part of the target holder. This work aims to characterize these tantalum-rich features and examine the mechanisms of impurity deposition.Plasma-induced surface morphology of the tantalum-rich surface layers depends on plasma properties and target temperature and chemistry. Greater titanium sputtering compared to zirconium resulted in more distinct surface features in the TiB2 samples compared to the ZrB2 samples via increased, prompt deposition onto tantalum surface impurities. There is still uncertainty as to why thick tantalum deposition only occurred under some plasma exposure conditions but not others; it is likely due to tantalum sputtering by a combination of boron molecules from the targets and carbon-impurities in the tantalum mask or targets. Impurity driven surface features are a well-documented phenomena in samples exposed to plasma from linear plasma device facilities—this work confirms the occurrence of this and emphasizes the need for chemistry characterization of isolated post-mortem surface features in plasma-exposed samples.

Nuckols, Lauren↗
NASA NTRS1977

The tantalum-cased tantalum capacitor

Tantalum-cased tantalum capacitors were tested with regard to temperature stability, capacitance ratio, surge current capabilities, shock, vibration, and thermal shock. They were found to be superior to the conventional wet slug tantalum capacitor cased in silver, since they are more resistant to sulfuric acid. The tantalum-cased tantalum capacitors are widely accepted for use in critical electronic equipment because of their excellent performance and reliability.

Moynihan, J. D.↗
NASA NTRS1965

Tantalum cathode improves electron-beam evaporation of tantalum

Tantalum cathode is used in assembly for electron beam evaporation of tantalum onto a substrate. The cathode and anode are made of pure tantalum rather than tungsten to prevent contamination of the tantalum film deposited on the substrate.

Source record↗
DOE OSTI2024

High-pressure synthesis and neutron scattering study of tantalum hydride TaH 1.23(5) and a tantalum polymorph with A15-type structure

A unique type of tantalum hydride was synthesized by exposing tantalum dihydride to the high hydrogen pressure of 9 GPa and a temperature of using toroid-type high-pressure chambers. The samples of this hydride were cooled down to 100 K, recovered to ambient pressure, and studied in a metastable state by hot extraction, powder x-ray and neutron diffraction, and inelastic neutron scattering. X-ray diffraction demonstrated that this hydride had an A15-type crystal structure of metal lattice (space group , Ta atoms at the 2a and 6c Wyckoff positions) and a lattice parameter of a = 5.150(5) Å at T = 85 K. The hydrogen content determined by hot extraction was H/Ta - 1.23(5). Hydrogen desorption during heating the sample in vacuum proceeded in two steps—first, Δ⁢H⁡/Ta=0.2 was desorbed at around -70 °⁢C, and then the rest of the hydrogen was desorbed between 100 ⁢°C and 390 ⁢°⁢C. The A⁢15-type metal lattice was preserved upon hydrogen removal, leaving a unique polymorph of tantalum. Neutron diffraction of A⁢15-TaH 1.23⁢(5) demonstrated that hydrogen atoms occupy the 24⁢k and 16⁢i Wyckoff sites in the crystal structure, and annealing at 250 K resulted in a decrease of the 24⁢k and an increase of the 16⁢i site occupancies. Inelastic neutron scattering revealed four vibrational modes in the fundamental band of A⁢15-TaH 1.23⁢(5) at 72, 135, 145, and 166 meV, the first three and the last one of which were tentatively assigned to the vibrations of H atoms at the 24⁢k and 16⁢i sites, respectively. No superconductivity was found in A⁢15-TaH 1.1 and hydrogen-free A15-Ta at temperatures down to 1.5 K.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Microstructurally-Inspired Strategies to Print Tantalum and Tantalum-Tungsten Alloys

The goal of this project is to investigate strategies to print tantalum and tantalum- tungsten alloys, which are notoriously difficult to print with consistent results because of the sensitivity of the properties to small concentrations of interstitial impurities (particularly oxygen) and microstructure, and hence to processing conditions. The ultimate tensile stress (UTS) for non-additively manufactured Ta as a function of temperature shows a stunning variation. In direct metal laser sintering (DMLS) Ta, a strong dependence of porosity, grain morphology and texture on processing conditions was found.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Tantalum Experiments in Fully-Reflected Water-Moderated Triangular-Pitched U(6.90)O 2 Fuel Rod Lattices (1.02 cm Pitch)

The United States (US) Department of Energy (DOE) Nuclear Energy Research Initiative funded the design and construction of the Seven Percent Critical Experiment (7uPCX) at Sandia National Laboratories (SNL). The start-up of the experiment facility and the execution of the experiments described here were funded by the DOE Nuclear Criticality Safety Program. The 7uPCX is designed to investigate critical systems with fuel for light water reactors in the enrichment range above 5 % 235 U. The 7uPCX assembly is a water moderated and — reflected array of aluminum-clad U(6.90 %)O 2 fuel rods. Other critical experiments performed in the 7uPCX assembly are documented in LEU-COMP-THERM-078, LEU-COMP-THERM-080, LEU-COMP-THERM 096, LEU- COMP-THERM-097, LEU-COMP-THERM-101, LEU-COMP-THERM-102, and LEU-COMP-THERM-111. Applied interests in neutron-absorbing elements at epithermal and intermediate neutron energy ranges at DOE’s Hanford Site and Savannah River Site were identified through DOE Office of Environmental Management (EM) workshops and needs surveys performed in conjunction with the National Nuclear Security Administration/Nuclear Criticality Safety Program. In response, a team lead by Oak Ridge National Laboratory (ORNL) performed a study evaluating the use of 7uPCX for testing the epithermal cross sections of materials at SNL. This marked the inception of the set of experiments described here. The purpose of these experiments was to measure the effects of tantalum in nearly-critical systems. The tantalum was introduced into the fuel arrays as experiment rods within a central test region. The central test region was designed to target the epithermal neutron energy range by providing a dry cylindrical cavity constructed of aluminum and lined with 0.04 in (0.1016 cm) thick cadmium sheet. The central test region has an outer diameter of 3.75 in (9.525 cm) length of 31 in (78.74 cm) and can hold 85 tantalum rods nominally 0.25 in (0.635 cm) outside diameter and 31.25 in (79.375 cm) long. The critical experiments were done using a set of triangular-pitched grid plates fabricated for these experiments. The grid plate set accommodated a fuel array of a total of 2016 fuel rod positions on a pitch of 0.4 in (1.016 cm) in a series of 21 hexagonal rings positioned around the central test region. The fuel used in these experiments was fabricated using unirradiated 6.90 % enriched UO 2 fuel pellets from fuel elements designed to be used in the internal nuclear superheater section of the Pathfinder boiling water reactor operated in South Dakota by the Northern States Power Company in the 1960s. The fuel elements were obtained from The Pennsylvania State University where they had been stored for many years. The fuel pellets in those fuel elements were removed from the original Incoloy cladding and reclad in 3003 aluminum tubes and end caps for use in the experiments reported here. The eight cases in this experiment series were performed in 2024 in the Sandia Critical Experiments (SCX) at the Sandia Pulsed Reactor Facility by varying the number of fuel rods in the critical assembly. The personnel involved in conducting these experiments included David Ames, Elijah Lutz, Beth Hanson, Patrick Ward, Jason Soares, and Augie Chapa from SNL, as well as Mathieu Dupont and B.J. Marshall from ORNL. Case 1 had no tantalum experiment rods. Case 2 had seven tantalum rods in the center of the central test region. Case 3 had 18 tantalum rods in the third hexagonal ring of the central test region. Case 4 had 19 tantalum rods in the center of the central test region. Case 5 had 30 tantalum rods in the outer most positions of the central test region. Case 6 had 37 tantalum rods in the center of the central test region. Case 7 had 61 tantalum rods in the center of the central test region. Case 8 had 85 tantalum rods filling all positions in the central test region. All eight critical experiments are judged to be acceptable as benchmark experiments.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗
NASA NTRS1985

The effect of tantalum on the structure/properties of two polycrystalline nickel-base superalloys: B-1900 + Hf MAR-M247

The microstructure, phase compositions, and phase fractions were studied in conventionally cast B-1900 + Hf and both conventionally cast and directionally solidified MAR-M247 as a function of tantalum concentration. The hot tensile and creep rupture properties of the solutionized and aged MAR-M247-type alloys were also determined as a function of tantalum level. The effects of tantalum on the microstructure and phase compositions of B-1900 + Hf and MAR-M247 (conventionally cast and directionally solidified) were found to be very similar. The addition of tantalum to the as cast and heat treated alloys was shown to cause the partial replacement of the Hf in the MC carbides by Ta, although the degree of replacement was decreased by the solutionizing and aging heat treatment. The gamma prime and minor phase fractions (primarily MC type carbides) both increased approximately linearly with tantalum concentration. The gamma prime phase compositions were relatively insensitive to tantalum variations with the exception of the tantalum and/or hafnium levels. Bulk tantalum additions increased the tantalum, chromium, and cobalt levels of the gamma phase in both alloy series. The increase in the concentrations of the latter two elements in the gamma phase was a result of the decrease in the gamma phase fraction with increasing bulk tantalum concentration and constant gamma/gamma prime partitioning ratio. Tantalum additions increased the yield stress and ultimate tensile strength of the directionally solidified MAR-M247 type alloys and had no significant effect on ductility.

Janowski, G. M.↗
NASA NTRS1984

The effect of tantalum and carbon on the structure/properties of a single crystal nickel-base superalloy

The microstructure, phase chemistry, and creep and hot tensile properties were studied as a function of tantalum and carbon levels in Mar-M247 type single crystal alloys. Microstructural studies showed that several types of carbides (MC, M23C6 and M5C) are present in the normal carbon (0.10 wt % C) alloys after heat treatment. In general, the composition of the MC carbides changes from titanium rich to tantalum rich as the tantalum level in the alloy increases. Small M23C6 carbides are present in all alloys. Tungsten rich M6C carbides are also observed in the alloy containing no tantalum. No carbides are present in the low carbon (0.01 wt % C) alloy series. The morphology of gamma prime is observed to be sensitive to heat treatment and tantalum level in the alloy. Cuboidal gamma prime is present in all the as cast structures. After heat treatment, the gamma prime precipitates tend to have a more spheroidal like morphology, and this tendency increases as the tantalum level decreases. On prolonged aging, the gamma prime reverts back to a cuboidal morphology or under stress at high temperatures, forms a rafted structure. The weight fraction and lattice parameter of the spheroidal gamma prime increases with increasing tantalum content. Changes in the phase chemistry of the gamma prime matrix and gamma prime have also been analyzed using phase extraction techniques. The partitioning ratio decreases for tungsten and aluminum and increases for tantalum as the tantalum content increases for both alloy series; no significant changes occur in the partitioning ratios of the other alloying elements. A reduction in secondary creep rate and an increase in rupture time result from increasing the tantalum content and decreasing the carbon level.

Nguyen, H. C.↗
NASA NTRS2011

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.↗
NASA NTRS2007

Reliability Effects of Surge Current Testing of Solid Tantalum Capacitors

Solid tantalum capacitors are widely used in space applications to filter low-frequency ripple currents in power supply circuits and stabilize DC voltages in the system. Tantalum capacitors manufactured per military specifications (MIL-PRF-55365) are established reliability components and have less than 0.001% of failures per 1000 hours (the failure rate is less than 10 FIT) for grades D or S, thus positioning these parts among electronic components with the highest reliability characteristics. Still, failures of tantalum capacitors do happen and when it occurs it might have catastrophic consequences for the system. This is due to a short-circuit failure mode, which might be damaging to a power supply, and also to the capability of tantalum capacitors with manganese cathodes to self-ignite when a failure occurs in low-impedance applications. During such a failure, a substantial amount of energy is released by exothermic reaction of the tantalum pellet with oxygen generated by the overheated manganese oxide cathode, resulting not only in destruction of the part, but also in damage of the board and surrounding components. A specific feature of tantalum capacitors, compared to ceramic parts, is a relatively large value of capacitance, which in contemporary low-size chip capacitors reaches dozens and hundreds of microfarads. This might result in so-called surge current or turn-on failures in the parts when the board is first powered up. Such a failure, which is considered as the most prevalent type of failures in tantalum capacitors [I], is due to fast changes of the voltage in the circuit, dV/dt, producing high surge current spikes, I(sub sp) = Cx(dV/dt), when current in the circuit is unrestricted. These spikes can reach hundreds of amperes and cause catastrophic failures in the system. The mechanism of surge current failures has not been understood completely yet, and different hypotheses were discussed in relevant literature. These include a sustained scintillation breakdown model [1-3]; electrical oscillations in circuits with a relatively high inductance [4-6]; local overheating of the cathode [5,7, 8]; mechanical damage to tantalum pentoxide dielectric caused by the impact of MnO2 crystals [2,9, 10]; or stress-induced-generation of electron traps caused by electromagnetic forces developed during current spikes [11]. A commonly accepted explanation of the surge current failures is that at unlimited current supply during surge current conditions, the self-healing mechanism in tantalum capacitors does not work, and what would be a minor scintillation spike if the current were limited, becomes a catastrophic failure of the part [l, 12]. However, our data show that the scintillation breakdown voltages are significantly greater that the surge current breakdown voltages, so it is still not clear why the part, which has no scintillations, would fail at the same voltage during surge current testing (SCT).

Teverovsky, Alexander↗
NASA NTRS2015

Use of a Tantalum Liner to Reduce Bore Erosion and Increase Muzzle Velocity in Two-Stage Light Gas Guns

Muzzle velocities and gun erosion predicted by earlier numerical simulations of two stage light gas guns with steel gun tubes were in good agreement with experimental values. In a subsequent study, simulations of high performance shots were repeated with rhenium (Re) gun tubes. Large increases in muzzle velocity (2 - 4 km/sec) were predicted for Re tubes. In addition, the hydrogen-produced gun tube erosion was, in general, predicted to be zero with Re tubes. Tantalum (Ta) has some mechanical properties superior to those of Re. Tantalum has a lower modulus of elasticity than Re for better force transmission from the refractory metal liner to an underlying thick wall steel tube. Tantalum also has greater ductility than Re for better survivability during severe stress/strain cycles. Also, tantalum has been used as a coating or liner in military powder guns with encouraging results. Tantalum has, however, somewhat inferior thermal properties to those of rhenium, with a lower melting point and lower density and thermal conductivity. The present study was undertaken to see to what degree the muzzle velocity gains of rhenium gun tubes (over steel tubes) could be achieved with tantalum gun tubes. Nine high performance shots were modeled with a new version of our CFD gun code for steel, rhenium and tantalum gun tubes. For all except the highest velocity shot, the results with Ta tubes were nearly identical with those for Re tubes. Even for the highest velocity shot, the muzzle velocity gain over a steel tube using Ta was 82% of the gain obtained using Re. Thus, the somewhat inferior thermal properties of Ta (when compared to those of Re) translate into only very slightly poorer overall muzzle velocity performance. When this fact is combined with the superior mechanical properties of Ta and the encouraging performance of Ta liners/coatings in military powder guns, tantalum is to be preferred over Re as a liner/coating material for two stage light gas guns to increase muzzle velocity and reduce bore erosion.

Launchers↗
NASA NTRS2021

Effect of Soldering on Polymer and MnO2 Tantalum Capacitors

Soldering might have a strong effect on performance and reliability of most surface mount technology components, including tantalum capacitors. High quality tantalum capacitors are likely the only type of components where soldering simulation is the first step during screening. Nevertheless, post-soldering failures of tantalum capacitors happen and require additional analysis. Popcorning is a well-known effect in plastic encapsulated microcircuits (PEM) and it occurs also in chip tantalum capacitors. The sensitivity of parts to the presence of moisture during soldering is characterized by the moisture sensitivity level (MSL); however, contrary to PEMs, there is no standard procedure for establishing MSL for tantalum capacitors. The effect of absorbed moisture on soldering related degradation and failures in tantalum capacitors have not been studied properly yet, and there is no sufficient information regarding the difference in the sensitivity to soldering between polymer and MnO2 tantalum capacitors. In this work, 16 types of polymer and 9 types of MnO2 cathodes tantalum capacitors with different moisture content have been tested before and after reflow soldering. The level of moisture release after soldering has been estimated and thermo-mechanical analysis used to assess deformation of capacitors during soldering simulations. Results show that moisture uptake in similar parts is approximately two times greater in polymer than in MnO2 capacitors. Cracking of the case and degradation of parameters can occur in both types of parts, but MnO2 capacitors are much more likely to fail catastrophically with a short circuit and possible ignition during the first power-on cycle. This type of failure in MnO2 capacitors is lot-related, can occur even at derated voltages and relatively low levels of moisture sorption corresponding to room conditions. Baking before soldering is an effective measure to prevent failures even in lots susceptible to popcorning damage. Recommendations for baking and testing to establish MSL are suggested.

Alexander Teverovsky↗
NASA NTRS2021

Effect of Preconditioning on Post-Soldering Failures in Tantalum Capacitors

Soldering have a strong effect on performance and reliability of most surface mount technology components, including tantalum capacitors. High quality tantalum capacitors are likely the only type of components where soldering simulation is the first step during screening. Nevertheless, post-soldering failures of tantalum capacitors do happen and require additional analysis. Popcorning is a well-known effect in plastic encapsulated microcircuits (PEM) and it occurs also in chip tantalum capacitors. The sensitivity of parts to the presence of moisture during soldering is characterized by the moisture sensitivity level (MSL); however, contrary to PEMs, there is no standard procedure for establishing MSL for tantalum capacitors, and standard J-STD-020 is applicable partially only. In this work, the effect of absorbed moisture on soldering related degradation and failures in tantalum capacitors have been studied using 22 types of polymer and 11 types of MnO2 cathodes tantalum capacitors including single and multianode parts. The amount of moisture released during soldering has been estimated by measurements of mass and capacitance variations. Results show that moisture uptake in similar parts is approximately two times greater in polymer than in MnO2 capacitors. Cracking of the case and degradation of parameters can occur in both types of parts, but MnO2 capacitors are much more susceptible to catastrophic short circuit failures and their ignition is possible during the first power-on cycle. This type of failure in MnO2 capacitors is lot-related, can occur even at derated voltages and relatively low levels of moisture sorption corresponding to room conditions. Baking before soldering is an effective measure to prevent failures even in lots susceptible to popcorning damage. Recommendations for testing to establish MSL and for baking to reduce the probability of failures are suggested.

tantalum polymer capacitors↗
DOE OSTI2025

Chemical Analysis of Tantalum Thin Films compared to Niobium Thin Films using SIMS and XPS

Superconducting qubits are a leading platform for quantum computation. These circuits are typically made from superconducting materials like aluminum or niobium. However, the amorphous niobium oxide and aluminum oxide on the surface of these circuits introduce considerable RF loss due to the presence of two-level systems (TLS), which limits the maximum coherence times T1 to ~100 μs. Capping the niobium qubits with a tantalum layer leads to a 3- 5x improvement [Bal et al., 2024]. But even in this case, tantalum forms an amorphous surface oxide that introduces loss. In an effort to devise strategies to eliminate the presence of this oxide, we present a comprehensive study on the nature of Ta oxide using x-ray photoemission spectroscopy (XPS) and secondary ion mass spectrometry (ToF-SIMS) as a function of heat treatment. The thin films were annealed in ultra-high vacuum conditions and analyzed in situ to characterize the composition and evolution of the native tantalum oxide layer and oxide-metal interface. Our analysis reveals two critical differences between tantalum and niobium oxides: Nb2O5 completely dissolves at 400°C, while Ta2O5 persists even at 800°C. Additionally, tantalum oxide contains only a single suboxide (TaO), in contrast to niobium's two suboxides (NbO and NbO2). The suboxide of tantalum contributes minimally to the total oxide content and shows a relative increase with temperature. Understanding the oxide’s behavior will open new pathways for optimizing coherence times in tantalum qubits.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗
DOE OSTI2025

Supply Chain Improvement & Process Modification Printing in Tantalum

Refractory metals and alloys are distinguished by their exceptional thermophysical properties, including high melting and recrystallization temperatures, remarkable strength, and superior corrosion resistance, all of which surpass those of conventional alloys. These unique characteristics position these materials as ideal candidates for applications in extreme environments. However, their potential has historically been underexploited due to limitations in processing capabilities. Recent advancements in melt-based additive manufacturing (AM) processes present opportunities to overcome these limitations. Previous Sandia studies have successfully characterized pure tantalum produced through laser powder bed fusion (LPBF) externally at Castheon, revealing that LPBF-fabricated tantalum exhibits properties exceeding those of wrought materials. This promising outcome sparked increased interest in the internal additive manufacturing of tantalum. This project aimed to establish the new SLM 280 machine at SNL-CA to successfully produce the first tantalum prints and characterize the material. Additionally, efforts were made to enhance the machine by incorporating Inert equipment to minimize oxygen content within the print volume. The results demonstrated that internally manufactured LPBF tantalum not only met but exceeded the standards of wrought materials, even prior to the integration of the additional equipment. The inert equipment is almost successfully integrated and ready for use. Future research should focus on understanding how this equipment influences the process-structure-property relationships, as well as further optimizing the printing parameters for tantalum.

36 MATERIALS SCIENCE↗