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At least 37 records · Page 2

Investigation of In Situ and Ex Situ Passivation of Pyrophoric Uranium–Niobium Alloy Powder

This work evaluates the effectiveness of in situ and ex situ passivation methods for mitigating the pyrophoricity of uranium–6 wt.% niobium spherical powders produced via the hydride–dehydride process coupled with plasma spheroidization. Oxide layer thickness was characterized using STEM/EDX, and pyrophoricity was assessed by a UN-recommended test method, which involves directly dropping the powders in the air. In situ passivation, performed by introducing flowing oxygen during spheroidization, produced oxide layers ranging from tens to hundreds of nanometers but resulted in inconsistent pyrophoricity mitigation at lower oxygen flow rates. Ex situ passivation, achieved by slow oxygen exposure over several months, formed uniform oxide layers of approximately 20 nm and consistently mitigated pyrophoricity. Despite requiring higher bulk oxygen content, in situ passivation enables faster processing and control of oxygen, while ex situ passivation achieves superior oxide uniformity with lower oxygen incorporation. These findings highlight the trade-offs between passivation methods and provide a foundation for improving the safety and scalability of reactive metal powder production.

U-6Nb↗

Long-time creep behavior of the niobium alloy C-103

The creep behavior of C-103 was studied as a function of stress, temperature, and grain size for test times to 19000 hr. Over the temperature range 827 to 1204 C and the stress range 6.89 to 138 MPa, only tertiary (accelerating) creep was observed. The creep strain epsilon can be related to time t by an exponential relation epsilon = epsilon(0) + K e raised to power (st) - 1), where epsilon (0) is initial creep strain, K is the tertiary creep strain parameter, and s is the tertiary creep rate parameter. The observed stress exponent 2.87 is similar to the three power law generally observed for secondary (linear) creep of Class I solid solutions. The apparent activation energy 374 kj/g mol is close to that observed for self diffusion of pure niobium. The initial tertiary creep rate was slightly faster for fine grained than for coarse-grained material. The strain parameter K can be expressed as a combination of power functions of stress and grain size and an exponential function of temperature. Strain time curves generated by using calculated values for K and s showed reasonable agreement with observed curves to strains of at least 4 percent. The time to 1 percent strain was related to stress, temperature, and grain size in a similar manner as the initial tertiary creep rate.

Titran, R. H.↗

Rapid method for determining nitrogen in tantalum and niobium alloys

Adaptation of commercial instrument which measures nitrogen and oxygen in steel gave results in less than four minutes. Sample is heated in helium atmosphere in single-use graphite crucible. Platinum flux facilitates melting of sample. Released gases are separated chromatographically and measured in thermal-conductivity cell.

Merkle, E. J.↗

Preliminary study of niobium alloy contamination by transport through helium

Preliminary tests were conducted to determine if interstitial element transport through a circulating helium working fluid was a potential problem in Brayton and Stirling space power systems. Test specimens exposed to a thermal gradient for up to 3000-hr included Nb-1%Zr, a Sm-Co alloy (referred to as SmCo in this paper), Hiperco 50 steel, and alumina to simulate various engine components of the Brayton and Stirling systems. Results indicate that helium transport of interstitial contaminants can be minimized over a 7-yr life with a monometallic Nb-1%Zr design. Exposure with other materials indicated a potential for interstitial contaminant transport. Determination of contamination kinetics and the effects on structural integrity will require additional testing.

Scheuermann, Coulson M.↗

Creep behavior of niobium alloy PWC-11

The high vacuum creep and creep-rupture behavior of a Nb-1Zr-.1C alloy (PWC 11) was investigated at 1350 and 1400 K with an applied stress of 40 MPa. The material was tested in the following four conditions: annealed (1 hr 1755 K/2 hr 1475 K); annealed plus EB welded; annealed plus aged for 1000 hr at 1350 or 1400 K; and annealed, welded, and aged. It was found that the material in the annealed state was the most creep-resistant condition tested, and that aging the alloy for 1000 hr without an applied stress greatly reduced that strength; however, it was still approximately three times as creep resistant as Nb-1Zr. Additionally, the EB weld region was stronger than the base metal in each condition tested, and phase extraction of the dispersed precipitate revealed the presence of a 70%ZrC-30%NbC cubic monocarbide phase.

Titran, R. H.↗

Preliminary study of niobium alloy contamination by transport through helium

Transport of gaseous contaminants through the working fluid to or from sensitive refractory alloys is theoretically possible during long time operation of Brayton and Stirling space power generation systems which use a gas as the working fluid. A test was designed which could give an answer to whether transport of contaminants through the working fluid was a potential major problem. The findings of that preliminary study are summarized.

Scheuermann, C. M.↗

Creep strength of niobium alloys, Nb-1%Zr and PWC-11

A study is being conducted at NASA Lewis Research Center to determine the feasibility of using a carbide particle strengthened Nb-1 percent Zr base alloy to meet the anticipated temperature and creep resistance requirements of proposed near term space power systems. In order to provide information to aid in the determination of the suitability of the PWC-11 alloy as an alternative to Nb-1 percent Zr in space power systems this study investigated: (1) the long-time high-vacuum creep behavior of the PWC-11 material and the Nb-1 percent Zr alloy, (2) the effect of prior stress-free thermal aging on this creep behavior, (3) the effect of electron beam (EB) welding on this creep behavior, and (4) the stability of creep strengthening carbide particles.

Titran, Robert H.↗

ULTIMATE Phase I project: Development of Niobium-based alloys for Turbine Applications

Current Ni-based alloys used in turbine blade applications are operating at 1100°C which is approximately 90% of the solidus of Ni-based alloys. Further increases in temperature can be achieved only through the use of alloys with higher solidus temperatures such as refractory alloys which include Mo, Nb, W, Ta alloys. Niobium has a unique combination of physical properties that include a high melting point (2468°C), lowest density (8.57 g/cc), and the lowest modulus amongst refractory alloys, a good thermal conductivity that increases from 45 W/mK at room temperature to 62 W/mK at 1093°C, good ductility with fabricability using traditional techniques, high strength, good creep resistance, and general chemical inactivity. Hence niobium alloys offer many advantages for use at the desired temperature of 1300°C. One of the major deterrents to the use of niobium and its alloys at high temperatures is achieving good oxidation resistance. In addition, achieving balanced properties of room temperature strength, ductility, fracture toughness, high temperature strength, and creep resistance required for 1300°C operation at a density of 9 g/cm 3 is extremely challenging since the addition of W which is a potent strengthener increases the density of the alloy. This project seeks to enable the development of a tri-layered turbine blade that can operate continuously at 1300°C with the core of the turbine blade providing good creep resistance, the second layer providing improved oxidation resistance over the core layer, and the third layer being an environmental barrier providing oxidation resistance. The objective of this Phase 1 project was to use computational modeling and advanced characterization tools to develop two classes of Nb alloys which could be used as the core layer and the transition layer. The first class of alloys developed in this project was a Nb-alloy designed to serve as the turbine blade core with excellent room temperature strength, ductility, and high temperature strength and creep resistance required for 1300°C operation. These alloys were designed to contain sufficient solute solution strengthening elements (W, Mo) but constrained by the density of alloy, along with the addition of elements such as Zr, Hf, Ta, C, and N to achieve a combination of primary and secondary carbide precipitation. A total of 38 “creep-resistant” alloys were designed and cast during the duration of the project. Processing techniques were developed to keep the oxygen contents as low as possible with typical oxygen contents less than 250 ppm. One alloy with a density of < 9.5 g/cc was successful in meeting the Phase 2 intermediate project mechanical property milestone requirements of room temperature ductility greater than 1.0%, 1200°C creep strain of less than 3% at 150 MPa and 100 hours in vacuum, and with solidus temperature greater than 1500ᵒC. The second class of alloys was designed to be a Nb-rich alloy with improved oxidation resistance when compared to the core layer and was designed specifically to be compatible with the core layer and the outer environmental barrier coating. This Nb- alloy will be specifically designed to be microstructurally stable at these temperatures when in contact with the core alloy and provide protection against catastrophic failure of the barrier coating. Two alloys were cast and processed but further development was discontinued to focus on the development of the creep resistant alloy.

36 MATERIALS SCIENCE↗

Development of Niobium-based alloys for Turbine Applications: 20/CJ000/08/09 (ULTIMATE Phase I project)

Current Ni-based alloys used in turbine blade applications are operating at 1100°C which is approximately 90% of the solidus of Ni-based alloys. Further increases in temperature can be achieved only through the use of alloys with higher solidus temperatures such as refractory alloys which include Mo, Nb, W, Ta alloys. Niobium has a unique combination of physical properties that include a high melting point (2468°C), lowest density (8.57 g/cc), and the lowest modulus amongst refractory alloys, a good thermal conductivity that increases from 45 W/mK at room temperature to 62 W/mK at 1093°C, good ductility with fabricability using traditional techniques, high strength, good creep resistance, and general chemical inactivity. Hence niobium alloys offer many advantages for use at the desired temperature of 1300°C. One of the major deterrents to the use of niobium and its alloys at high temperatures is achieving good oxidation resistance. In addition, achieving balanced properties of room temperature strength, ductility, fracture toughness, high temperature strength, and creep resistance required for 1300°C operation at a density of 9 g/cm 3 is extremely challenging since the addition of W which is a potent strengthener increases the density of the alloy. This project seeks to enable the development of a tri-layered turbine blade that can operate continuously at 1300°C with the core of the turbine blade providing good creep resistance, the second layer providing improved oxidation resistance over the core layer, and the third layer being an environmental barrier providing oxidation resistance. The objective of this Phase 1 project was to use computational modeling and advanced characterization tools to develop two classes of Nb alloys which could be used as the core layer and the transition layer.

36 MATERIALS SCIENCE↗

Copper-acrylic enamel serves as lubricant for cold drawing of refractory metals

Acrylic enamel spray containing metallic copper pigment lubricates refractory metal tubing during cold drawing operations so that the tubing surface remains free from scratches and nicks and does not seize in the die. Zirconium alloys, zirconium, tantalum alloys, niobium alloys, vanandium alloys and titanium alloys have been drawn using this lubricant.

Beane, C.↗

Characterization of precipitates in a niobium-zirconium-carbon alloy

A niobium alloy with 1 percent zirconium and 0.063 percent carbon by weight was investigated in the as-rolled and annealed conditions, and after high-temperature (1350 and 1400 K) exposure with and without an applied stress. In the as-rolled and annealed conditions, large metastable carbides were observed in addition to a regular distribution of small particles. During the high-temperature exposure, the majority of the large carbides were dissolved and a more stable carbide phase formed. This finely dispersed phase had a composition determined to be approximately 70 percent ZrC and approximately 30 percent NbC and showed some evidence of an orientation relationship with the matrix. The precipitates appeared to coarsen slightly after approximately 5000 hr exposure in the presence of an applied stress resulted in a decrease in the size and in the interparticle spacing of the stable precipitates. However, the composition of the precipitate phase and its ability to pin dislocations were not affected by the temperature or stress conditions.

Grobstein, T. L.↗

Short-Term Elevated Temperature Mechanical Performance and Microstructure of A Niobium-Zirconium Alloy Produced via Laser Powder Bed Fusion In-Situ Alloying

Nb-1Zr is a readily fabricable, dispersion-strengthened niobium alloy with improved elevated temperature properties compared to commercially pure niobium. This low to moderate strength niobium alloy is desirable in thermal management systems for fission power and propulsion applications; however, pre-alloyed spherical feedstock for powder-based additive manufacturing processes is generally unavailable. Laser powder bed fusion (L-PBF) in-situ alloying of a Nb-1Zr chemistry was performed using a high-purity niobium feedstock coated with 1 wt% of zirconium-based ceramic compound nano-powders: ZrO 2 , ZrC, and ZrH 2 . The additively manufactured material was mechanically tested at elevated temperatures within a controlled environment in the as-built condition. For comparison, traditionally manufactured wrought feedstock was also tested within an identical environment. Examination of the materials’ microstructure and short-term elevated temperature mechanical response determined: in-situ alloying of spherical Nb powder feedstock with Zr-based ceramic nanoparticles can be successfully implemented; the ZrO 2 addition offered the greatest elevated temperature stability and strength but exhibited brittle behavior; the ZrC addition achieved a balance of room temperature ductility and elevated temperature strength; and the ZrH 2 -modified material had the lowest as-built interstitial content and showed high ductility with mechanical performance most similar to wrought Nb-1Zr.

Niobium Alloy↗

List of Commercial and Advanced Developmental Niobium-Based Alloys of the Space Age

This report compiles a list of commercial and developmental niobium-based alloys developed during the Space Age (late 1950s through mid-1970s) for extreme-temperature applications, including rocket engine thrust chambers, hypersonic re-entry thermal protection systems, and space fission reactor loops. Niobium (Nb) was widely pursued because it provided the lowest density (~8.6 g/cc) among the primary refractory metals, a high melting temperature (~2470°C), exceptional low-temperature ductility, good formability, and compatibility with liquid alkali metals. An evaluation of physical metallurgy mechanisms, focusing on solid-solution strengthening via heavy refractory solutes (W, Mo, Ta), dual-purpose reactive solutes (Hf, Zr, Ti), and dispersion strengthening using carbides, nitrides, and oxides is presented. Additionally, the report compares Western and Soviet Union metallurgical approaches, explaining how supply chain factors and manufacturing infrastructure influenced element selection, interstitial chemistry, and alloy identification/naming conventions. Cataloging these historical alloy chemical compositions serves as a foundational reference for modern alloy additive manufacturing, thermodynamic CALPHAD modeling, and machine-learning discovery pipelines for next-generation extreme-environment niobium-based alloys.

Physical Metallurgy↗