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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 19 records

Exploration of alloy surface and slurry modification to improve oxidation life of fused silicide coated niobium alloys

Edge and surface modifications of niobium alloys were investigated prior to coating with Si-20Cr-20Fe and slurry composition modification for performance in a 1370 C ambient pressure slow cycle test. The best coating obtained was Si-20Cr-20Mn with an average life of 63 cycles, compared to 40 for Si-20Cr-20Fe on FS-85 (100 percent improvement in weight parity life). Edge beading extended the lives of Si-20Cr-20Fe-coated Cb-752 and FS-85 to 57 and 41 cycles respectively (50 and 20 percent improvements in weight parity life respectively). W, Al2O3 and ZrO2(CaO) surface modifications altered coating crack frequency and microstructure and increased life somewhat.

Levine, S. R.↗

Exploration of alloy surface and slurry modification to improve oxidation life of fused silicide coated niobium alloys.

Edge and surface modification of niobium alloys prior to coating with Si-20Cr-20Fe and slurry composition modification were investigated to improve performance in a 1370 C, ambient pressure, slow-cycle test. The best coating obtained was Si-20Cr-20Mn with an average life of 63 cycles compared to 40 for Si-20Cr-20Fe on FS-85 (100 percent improvement in weight parity life). Edge beading extended the lives of Si-20Cr-20Fe coated Cb-752 and FS-85 to 57 and 41 cycles, respectively (50 and 20 percent improvements in weight parity life, respectively).

Levine, S. R.↗

Electron Beam Melting of Niobium Alloys from Blended Powders

Niobium-based tungsten alloys are desirable for high-temperature structural applications yet are restricted in practice by limited room-temperature ductility and fabricability. Powder bed fusion additive manufacturing is one technology that could be leveraged to process alloys with limited ductility, without the need for pre-alloying. A custom electron beam powder bed fusion machine was used to demonstrate the processability of blended Nb-1Zr, Nb-10W-1Zr-0.1C, and Nb-20W-1Zr-0.1C powders, with resulting solid optical densities of 99+%. Ultimately, post-processing heat treatments were required to increase tungsten diffusion in niobium, as well as to attain satisfactory mechanical properties.

36 MATERIALS SCIENCE↗

Electron Beam Welding of Additively Manufactured Niobium Alloy Heat Pipes

Additively manufactured refractory alloy-liquid metal heat pipes are being developed and tested for thermal management systems within nuclear propulsion and power applications. This study investigated electron beam (EB) welded joints on a laser powder bed fusion printed niobium alloy (C-103) and the impact of multiple joined heat pipe sections on working fluid flow and container leak-tightness. Results showed that EB welded joints connecting multiple heat pipe sections do not impact working fluid wicking behavior and the printed C-103 material and the EB welds joining the tubular sections created a leak-tight container. Interestingly, CT data showed an order of magnitude greater number and volume of porosity indications in the ground mating surface weld compared to the as-printed mating surface weld. The work concluded that AM is a viable manufacturing process for niobium alloy heat pipes and provided valuable insights for future AM heat pipe research and development.

Electron beam welding↗

Reactive Melt Infiltration of Silicon-Niobium Alloys in Microporous Carbons

Studies of the reactive melt infiltration of silicon-niobium alloys in microporous carbon preforms prepared by the pyrolysis of a polymer precursor have been carried out using modeling, Differential Thermal Analysis (DTA), and melt infiltration. Mercury porosimetry results indicate a very narrow pore size distribution with virtually all the porosity within the carbon preforms open to infiltrants. The morphology and amount of the residual phases (niobium disilicide and silicon) in the infiltrated material can be tailored according to requirements by careful control of the properties (pore size and pore volume) of the porous carbon preforms and alloy composition. The average room temperature four-point flexural strength of a reaction-formed silicon carbide material (made by the infiltration of medium pore size carbon preform with Si - 5 at. % Nb alloy) is 290 +/- 40 MPa (42 +/- 6 ksi) and the fracture toughness is 3.7 +/- 0.3 MPa square root of m. The flexural strength decreases at high temperatures due to relaxation of residual thermal stresses and the presence of free silicon in the material.

Singh, M.↗

A Dispersion-Strengthened Low-Density Niobium Alloy and Its Elevated Temperature Mechanical Performance

In response to the elevated-temperature and weight-reduction demands of modern aerospace applications, a novel oxide-dispersion-strengthened low-density niobium alloy (LDNb-ODS) was fabricated using laser powder bed fusion (L-PBF). To overcome powder procurement barriers, L-PBF feedstock was produced by blending commercial Nb521, Ti64, and Cr powder with Y2O3 nanoparticles via resonant acoustic mixing. Following L-PBF and a 1400°C vacuum heat treatment, the alloy achieved a density of 6.73 g/cc and a fine mean grain size of 4.62 µm stabilized by uniform ~30 nm yttria dispersoids. Microstructural analysis revealed a chemically inhomogeneous build with lack-of-fusion defects and a titanium (Ti) shift from a nominal 31.5 wt% in the starting powder blend to 24.8 wt% in the printed part due to preferential Ti loss during printing. Elevated-temperature tensile testing demonstrated that LDNb-ODS maintained a superior specific yield strength of 60-85 MPa/(g/cc) up to 800°C, outperforming nickel-based alloys Ni625, Ni230, and GRX-810. Between 870°C and 950°C, its specific strength surpassed both Ni718 and Ni625. In rapid stress-rupture testing at 1093°C and 20.7 MPa, uncoated LDNb-ODS survived 21.4 hours (a tenfold increase over legacy C-103) while an R512E silicide coating extended rupture life to 84.8 hours, confirming that oxidation accelerates low-stress failure. These findings demonstrate that additive manufacturing of LDNb-ODS provides a viable, lightweight alternative to nickel-based superalloys for high-temperature (>850°C) aerospace components.

Low Density Niobium Alloy↗

The lattice parameter – composition relationship of the body centered cubic uranium-niobium alloys

In this paper, in-situ time-of-flight neutron diffraction experiments were performed on uranium-niobium alloy with 6 wt% Nb to study the lattice parameter-composition relationship for the body centered cubic (bcc) alloys. Based on lattice-parameter measurements of Nb-supersaturated γs phase over the range of 450 – 790 °C, an improved Vegard's-type relationship was established for determination of Nb concentrations at elevated temperatures. Neutron diffraction data were also collected as a function of aging time over the 450 - 600 °C range when γs phase decomposed isothermally into the mixture of orthorhombic α-U and Nb-rich bcc phase, as well as at room-temperature on the alloys aged ex-situ at 500 °C up to five years. From these measurements, the average Nb concentrations in the bcc phase were determined based on the Rietveld refinements of weight fraction and mass conservation relations (lever rule). Over the 15at% – 78at% range of Nb concentrations that correspond to different experimental aging times, the lattice parameters at constant temperatures exhibit a nonlinear S-shaped variation with Nb concentration, and the associated excess volumes of mixing can be described by a subregular solution model of the Redlich–Kister type of polynomial. Over the full range of composition the S-shaped deviation from Vegard's law can be modeled using a combination of an elastic continuum model and a perturbation to the radii of the solute atoms in the solvent, suggesting that electronic interactions between solute and solvent atoms could play an important role in the compositional dependence of lattice parameter for the γ-phase U-Nb alloys. While Vegard's law is a straightforward and reasonably good approximation for the bcc solid solutions in the U-Nb system, the Nb concentrations determined from the weight fraction refinements of diffraction data provide internally consistent, mass-conserving estimates of solute redistribution for the monotectoid reaction.

36 MATERIALS SCIENCE↗

Compatibility of Niobium Alloys and Superalloys in a Flowing He-Xe Power Conversion System

Proposed concepts for an ambitious mission to explore Jupiter's three icy moons place significant demands on the various spacecraft systems. There are many challenges related to the high output power conversion systems being considered, and one example is the need to ensure system compatibility at all levels. The utilization of appropriate materials for component structures is important to ensuring long mission life. Refractory metal alloys have attractive high-temperature properties in inert environments, but these alloys are sometimes susceptible to contamination. Potential material compatibility issues exist between refractory metal candidates and more conventional alloys. Nb-1Zr has long been considered one of the most well characterized refractory alloys that is well suited for elevated-temperature use and liquid-metal compatibility. However, previous studies have suggested that niobium alloys can not co-exist in a closed system with traditional stainless steels or superalloys due to transport of contaminants. The relevance of this information to a proposed power conversion system is discussed. Also, experiments and fundamental calculations are being performed to determine contamination transport from candidate superalloys to Nb-1Zr in a closed system with an inert carrier gas. Potential protective schemes are explored to ensure system level compatibility between the refractory alloy Nb-1Zr and a nickel-based superalloy.

Bowman, Cheryl L.↗

Separation of protactinium from uranium-niobium alloys for 231 Pa– 235 U radiochronometry in nuclear forensic investigations

The isolation and purification of protactinium from uranium materials is essential for 231 Pa– 235 U radiochronometry, but separating Pa from uranium-niobium alloys, a common material in the nuclear fuel cycle, is challenging due to the chemical similarity of Pa and Nb. Here, in this work, we present three resin chromatography separation techniques for isolating Pa from U and Nb which were independently developed by three different laboratories through ad hoc adaptations of standard operating procedures. Our results underscore the need for and value of purification methods suitable for a diversity of uranium-based materials to ensure the operational readiness of nuclear forensics laboratories.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Oxidation Behavior of Binary Niobium Alloys

This investigation concludes a study to determine the effects of up to 25 atomic percent of 55 alloying additions on the oxidation characteristics of niobium. The alloys were evaluated by oxidizing in an air atmosphere for 4 hours at 1000 C and 2 hours at 1200 C. Titanium and chromium improved oxidation resistance at both evaluation conditions. Vanadium and aluminum improved oxidation resistance at 1000 C, even though the V scale tended to liquefy and the Al specimens became brittle and the scale powdery. Copper, cobalt, iron, and iridium improved oxidation resistance at 1200 C. Other investigations report tungsten and molybdenum are protective up to about 1000 C, and tantalum at 1100 C. The most important factor influencing the rate of oxidation was the ion size of the alloy additions. Ions slightly smaller than the Nb(5+) ion are soluble in the oxide lattice and tend to lower the compressive stresses in the bulk scale that lead to cracking. The solubility of the alloying addition also depends on the valence to some extent. All of the elements mentioned that improve the oxidation resistance of Nb fit this size criterion with the possible exception of Al, whose extremely small size in large concentrations would probably lead to the formation of a powdery scale. Maintenance of a crack-free bulk scale for as long as possible may contribute to the formation of a dark subscale that ultimately is rate- controlling in the oxidation process. The platinum-group metals, especially Ir, appear to protect by entrapment of the finely dispersed alloying element by the incoming Nb2O5 metal-oxide interface. This inert metallic Ir when alloyed in a sufficient amount with Yb appears to give a ductile phase dispersed in the brittle oxide. This scale would then flow more easily to relieve the large compressive stresses to delay cracking. Complex oxide formation (which both Ti and Zr tend to initiate) and valence effects, which probably change the vacancy concentration in the scale, are masked by the overriding tendency for a porous scale.

Barrett, Charles A.↗

Hardness behavior of binary and ternary niobium alloys at 77 and 300 K

An investigation was conducted to determine the effects of alloy additions of zirconium, hafnium, molybdenum, tungsten, rhenium, ruthenium, osmium, rhodium, and iridium on the hardness of niobium. Both binary and ternary alloys were investigated by means of hardness tests at 77 and 300 K. Results showed that atomic size misfit plays a dominant role in controlling the hardness of binary niobium alloys. Alloy softening, which occurred at dilute solute additions, is most likely due to an extrinsic mechanism involving interaction between solute elements and interstitial impurities.

Stephens, J. R.↗

Machine learning guided optimal composition selection of niobium alloys for high temperature applications

Nickel- and cobalt-based superalloys are commonly used as turbine materials for high-temperature applications. However, their maximum operating temperature is limited to about 1100 °C. Therefore, to improve turbine efficiency, current research is focused on designing materials that can withstand higher temperatures. Niobium-based alloys can be considered as promising candidates because of their exceptional properties at elevated temperatures. The conventional approach to alloy design relies on phase diagrams and structure–property data of limited alloys and extrapolates this information into unexplored compositional space. In this work, we harness machine learning and provide an efficient design strategy for finding promising niobium-based alloy compositions with high yield and ultimate tensile strength. Unlike standard composition-based features, we use domain knowledge-based custom features and achieve higher prediction accuracy. We apply Bayesian optimization to screen out novel Nb-based quaternary and quinary alloy compositions and find these compositions have superior predicted strength over a range of temperatures. We develop a detailed design flow and include Python programming code, which could be helpful for accelerating alloy design in a limited alloy data regime.

Mohanty, Trupti (ORCID:0000000342701430)↗

Hardness behavior of binary and ternary niobium alloys at 77 and 300 K

The effects of alloy additions of zirconium, hafnium, molybdenum, tungsten, rhenium, ruthenium, osmium, rhodium, and iridium on the hardness of niobium was determined. Both binary and ternary alloys were investigated by means of hardness tests at 77 K and 300 K. Results showed that atomic size misfit plays a dominant role in controlling hardness of binary niobium alloys. Alloy softening, which occurred at dilute solute additions, is most likely due to an extrinsic mechanism involving interaction between solute elements and interstitial impurities.

Stephens, J. R.↗

Comparison of inert-gas-fusion and modified Kjeldahl techniques for determination of nitrogen in niobium alloys

This report compares results obtained for the determination of nitrogen in a selected group of niobium-base alloys by the inert-gas-fusion and the Kjeldahl procedures. In the inert-gas-fusion procedure the sample is heated to approximately 2700 C in a helium atmosphere in a single-use graphite crucible. A platinum flux is used to facilitate melting of the sample. The Kjeldahl method consisted of a rapid decomposition with a mixture of hydrofluoric acid, phosphoric acid, and potassium chromate; distillation in the presence of sodium hydroxide; and highly sensitive spectrophotometry with nitroprusside-catalyzed indophenol. In the 30- to 80-ppm range, the relative standard deviation was 5 to 7 percent for the inert-gas-fusion procedure and 2 to 8 percent for the Kjeldahl procedure. The agreement of the nitrogen results obtained by the two techniques is considered satisfactory.

Merkle, E. J.↗

Tensile Property and Lifetime Prediction for Low-Temperature Aged Uranium-Niobium Alloys

Thermal aging models and lifetime predictions for uranium-niobium (U-Nb) alloys were created using an approach similar to those previously employed. Lifetime estimates for generic U-6Nb components were thus updated; the reported value being 800 years. This update represents a small change in lifetime vs. that of the 2012 assessment (540 years). This lifetime estimate emerged from consideration of several model fits specific to the aging datasets and properties chosen. Aging was quantified using quasi-static tensile properties measured on specimens artificially aged for up to 10 years. The major change relative to the most recent 2012 LANL assessment was that a more comprehensive body of U-Nb literature data was mined, in addition to being augmented by the latest LANL and UK AWE data. The tensile data compilation was published separately (LANL report LA-14493, December 2016). Recognizing the chemical banding of industrially produced U-6Nb, models were developed for the mid-range (6 wt.%) and extrema (4 and 8 wt.%) compositions. Lifetime estimates were calculated for all three alloy classes (4, 6, 8 wt.% nominal) and two measures of total tensile elongation (TE) to failure, namely TE-ext. — extensometer method, and TE-NCD — normalized crosshead displacement method. The conservative assumption was made that whichever composition (4, 6, or 8 wt.% Nb) and property (TE-ext or TE-NCD) was the first to cross the ductility failure threshold would limit the lifetime of the entire component. Tensile strength properties did not figure into the lifetime predictions, but could be useful as age-sensitive diagnostics and were also modeled. Of these, only first yield strength is expected to show a change at 40°C aging vs. time = 0 over the ~100-year timespan of engineering interest. Second yield strength evolves more slowly, and ultimate tensile strength slower still. Among all the models, the apparent activation energies for aging were mostly in the narrow 29– 37 kcal/mol range, which is close to that for diffusion of Nb in gamma-uranium. This agreement may be coincidental. The data from recent long-term aging studies substantially improved the model fit quality and robustness of the lifetimes. Appendices document sensitivity studies of the model fits and lifetimes with respect to using more limited datasets. These results highlight the limitations of relying solely on data from scattered literature studies and smaller datasets more generally.

36 MATERIALS SCIENCE↗

Tensile and creep properties of titanium-vanadium, titanium-molybdenum, and titanium-niobium alloys

Tensile and creep properties of experimental beta-titanium alloys were determined. Titanium-vanadium alloys had substantially greater tensile and creep strength than the titanium-niobium and titanium-molybdenum alloys tested. Specific tensile strengths of several titanium-vanadium-aluminum-silicon alloys were equivalent or superior to those of commercial titanium alloys to temperatures of 650 C. The Ti-50V-3Al-1Si alloy had the best balance of tensile strength, creep strength, and metallurgical stability. Its 500 C creep strength was far superior to that of a widely used commercial titanium alloy, Ti-6Al-4V, and almost equivalent to that of newly developed commercial titanium alloys.

Gray, H. R.↗