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DOE OSTI2021

Structure-Property Relationships of Additively Manufactured Ni-Nb Alloys [Slides]

In this work, scratch and nanoindentation testing was used to determine hardness, fracture toughness, strain rate sensitivity, and activation volumes on additively manufactured graded and uniform Ni-Nb bulk specimens. Characterization showed the presence of a two phase system consisting of Ni 3 Nb and Ni 6 Nb 7 intermetallics. Intermetallics were multimodal in nature, having grain and cell sizes spanning from a few nanometers to 10s of micrometers. The unique microstructure resulted in impressively high hardness, up to 20 GPa in the case of the compositionally graded sample. AM methods with surface deformation techniques are a useful way to rapidly probe material properties and alloy composition space.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Structure-Property Relationships of Additively Manufactured Ni-Nb Alloys [Slides]

36 MATERIALS SCIENCE↗

DOE OSTI2023

Topographic Evolution of Heat-Treated Nb Upon Electropolishing for SRF Applications

Surface finish plays an essential role in the performance of superconducting radio frequency cavities. Several surface treatments have been developed to reduce surface resistance at a moderate accelerating gradient. We investigated the effects of sequential electropolishing on samples vacuum heat-treated at 300 and 600 °C and N-doped Nb samples using atomic force microscopy. The N-doping process precipitates niobium nitrides within grains and, most notably, continuously and deeply along some grain boundaries. Upon electropolishing, the nitrides are preferentially removed leaving behind a topographically imperfect surface marked by relatively deep holes and grooves with low radius of curvature edges. The progression of magnetic field enhancement and superheating field suppression factors upon electropolishing were investigated using atomic force micrographs. While minor changes in magnetic field enhancement and superheating field suppression factors are observed for the 300 and 600 °C heat-treated Nb, substantial improvements are observed for N-doped Nb. In this system, the most severe topographic defects are the grain boundary grooves which substantially suppress the superheating field. We find that the severity of topographic defects is related to the N-doping process.

Lechner, Eric↗

DOE OSTI2025

First Results from A $Nb_3Sn$-Coated 1.5-Cell 650MHZ SRF Cavity for Cryogen-Free Industrial Accelerators

Fermilab is advancing the development of a compact, high-power electron beam accelerator using superconducting radio frequency (SRF) technology as a non-radioactive alternative to traditional radiological sources. The current design targets continuous-wave (CW) operation at \SI{1.6}{MeV} and \SI{20}{kW}. To ensure suitability for industrial environments, the system is being designed for cryogen-free operation, driving the adoption of a novel Nb$_3$Sn-coated 1.5-cell SRF cavity operating at \SI{650}{MHz}. This contribution reports on the fabrication, surface preparation, and Nb$_3$Sn coating process of the cavity, as well as first results from vertical test stand (VTS) measurements performed in a liquid helium bath. These initial tests mark a key milestone toward demonstrating the viability of conduction-cooled Nb$_3$Sn SRF cavities for industrial-scale deployment.

Tagdulang, Nikki Diala [Fermilab]↗

DOE OSTI2020

Carbide Formation in Refractory Mo 15 Nb 20 Re 15 Ta 30 W 20 Alloy under a Combined High-Pressure and High-Temperature Condition

In this work, the formation of carbide with the concertation of carbon at 0.1 at.% in refractory high-entropy alloy (RHEA) Mo 15 Nb 20 Re 15 Ta 30 W 20 was studied under both ambient and high-pressure high-temperature conditions. The x-ray diffraction of dilute carbon (C)-doped RHEA under ambient pressure showed that the phases and lattice constant of RHEA were not influenced by the addition of 0.1 at.% C. In contrast, C-doped RHEA showed unexpected phase formation and transformation under combined high-pressure and high-temperature conditions by resistively employing the heated diamond anvil cell (DAC) technique. The new FCC_L1 2 phase appeared at 6 GPa and 809 °C and preserved the ambient temperature and pressure. High-pressure and high-temperature promoted the formation of carbides Ta 3 C and Nb 3 C, which are stable and may further improve the mechanical performance of the dilute C-doped alloy Mo 15 Nb 20 Re 15 Ta 30 W 20 .

36 MATERIALS SCIENCE↗

DOE OSTI2022

Luminescence and Scintillation in the Niobium Doped Oxyfluoride Rb4Ge5O9F6:Nb

A new niobium-doped inorganic scintillating oxyfluoride, Rb4Ge5O9F6:Nb, was synthesized in single crystal form by high-temperature flux growth. The host structure, Rb4Ge5O9F6, crystallizes in the orthorhombic space group Pbcn with lattice parameters a = 6.98430(10) Å, b = 11.7265(2) Å, and c = 19.2732(3) Å, consisting of germanium oxyfluoride layers made up of Ge3O9 units connected by GeO3F3 octahedra. In its pure form, Rb4Ge5O9F6 shows neither luminescence nor scintillation but when doped with niobium, Rb4Ge5O9F6:Nb exhibits bright blue luminescence and scintillation. The isostructural doped structure, Rb4Ge5O9F6:Nb, crystallizes in the orthorhombic space group Pbcn with lattice parameters a = 6.9960(3) Å, b = 11.7464(6) Å, and c = 19.3341(9) Å. X-ray absorption near edge structure (XANES) and extended X-ray absorption fine structure (EXAFS) measurements suggest that the niobium is located in an octahedral coordination environment. Optical measurements inform us that the niobium dopant acts as the activator. The synthesis, structure, and optical properties are reported, including radioluminescence (RL) measurements under X-ray irradiation.

Carone, Darren (ORCID:0000000164014098)↗

DOE OSTI2025

Probing Non-Equilibrium Pair-Breaking and Quasiparticle Dynamics in Nb Superconducting Resonators Under Magnetic Fields

We conducted a comprehensive study of the non-equilibrium dynamics of Cooper pair breaking, quasiparticle (QP) generation, and relaxation in niobium (Nb) cut from superconducting radio-frequency (SRF) cavities, as well as various Nb resonator films from transmon qubits. Using ultrafast pump–probe spectroscopy, we were able to isolate the superconducting coherence and pair-breaking responses. Our results reveal both similarities and notable differences in the temperature- and magnetic-field-dependent dynamics of the SRF cavity and thin-film resonator samples. Moreover, femtosecond-resolved QP generation and relaxation under an applied magnetic field reveals a clear correlation between non-equilibrium QPs and the quality factor of resonators fabricated by using different deposition methods, such as DC sputtering and high-power impulse magnetron sputtering. These findings highlight the pivotal influence of fabrication techniques on the coherence and performance of Nb-based quantum devices, which are vital for applications in superconducting qubits and high-energy superconducting radio-frequency applications.

43 PARTICLE ACCELERATORS↗

DOE OSTI2024

Microstructural and Oxidation Effects of Nb Additions to U3Si2

U3Si2 is a long term, accident-tolerant nuclear fuel candidate for light-water reactors because of its superior thermal conductivity and increased uranium density when compared to traditional uranium dioxide (UO2). While reducing internal thermal stresses and increasing efficiency, U3Si2 exhibits energetic oxidation during certain off-normal and accident scenarios, which include coolant or steam exposure. To mitigate this, Nb is investigated as an alloy constituent to enhance corrosion resistance and increase mechanical strength. The work presented investigates the response of Nb-alloyed U3Si2 to steam atmospheres. A thermogravimetric analysis is conducted in flowing steam to T > 1000 °C to assess oxidation resistance. The phase characterization of as-melted, thermally annealed and post-oxidation compositions with up to 12 vol% Nb by powder X-ray diffraction, scanning electron microscopy, and energy dispersive spectroscopy is reported.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

NASA NTRS1986

Long-time creep behavior of Nb-1Zr alloy containing carbon

Creep tests were conducted on the Nb-1Zr base alloy with and without carbon. Testing was performed at 10 to the -6 MPa in the 1350 to 1400 K range. Creep times, to 1 percent strain, ranged from 60 to 6000 hr. All 1 percent creep data were filled by linear regression to a temperature compensating rate equation. The Nb-1Zr-0.06C alloy, tested in a weakened aged condition, appears to be four times as strong as the Nb-1Zr alloy.

Titran, R. H.↗

NASA NTRS1988

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.↗

NASA NTRS1989

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.↗

NASA NTRS1991

Containerless processing and rapid solidification of Nb-Si alloys in the niobium-rich eutectic range

Containerless processing and rapid solidification techniques were used to process Nb-Si alloys in the Nb-rich eutectic range. Electromagnetically levitated drops were melted and subsequently splat-quenched from different temperatures. A variety of eutectic morphologies was obtained as a function of the degree of superheating or undercooling of the drops prior to splatting. Metallic glass was observed only in drops quenched from above the melting temperature. Microstructures of splats deeply undercooled prior to quenching were very fine and uniform. These results are discussed in terms of classic nucleation theory concepts and the expected heat evolution at different regions of the splat during the rapid quenching process. The locations of the coupled-zone boundaries for the alpha-Nb + Nb3Si eutectic are also suggested.

Hofmeister, W. H.↗

NASA NTRS1991

Containerless processing and rapid solidification of Nb-Si alloys of hypereutectic composition

A combination of bulk undercooling in an electromagnetic levitation apparatus and splat quenching between two copper plates is used to process Nb-Si alloys in order to maximize rapid solidification conditions and minimize the effects of recalescence, with emphasis on the solidification of characteristics of alloys in the 21 to 27 at. pct Si range of composition. SEM and TEM as well as X-ray diffraction are used to characterize the microstructures of the processed samples. In the range of compositions studied, the splat-quenched drops always formed the tetragonal Nb3Si phase directly from the liquid. Drops solidified in the coil were characterized by the presence of the primary intermetallic Nb5Si3 and the absence of both peritectic Nb3Si and the equilibrium eutectic. In these cases, a metastable alpha-Nb + beta-Nb5Si3 eutectic formed. The results are discussed in terms of possible metastable configurations of the Nb-Si phase diagram as well as concepts of nucleation and growth kinetics applied to the Nb3Si and Nb5Si3 intermetallics.

Hofmeister, W. H.↗

NASA NTRS1992

A new ordered tetragonal phase in the Ti3Al+Nb system

Results are reported from an experimental study of phase stability in a plasma-sprayed Ti3Al+Nb alloy using TEM and electron diffraction techniques. The alloys was produced from Ti3Al+Nb powder via an inductively coupled plasma deposition process. Evidence was found for the ordering of the B2 phase to a structure similar to the DO3-type phase, but with a tetragonal distortion. An ordered tetragonal phase (T) is proposed to account for these observations, and the existence of the B2 - T ordering transformation in the Ti3Al+Nb system is suggested. The T phase can be regarded as a DO3-like phase with a tetragonal distortion. The tegragonality c0/a0 is approximately equal to 1.02, and a0 equals 0.65 +/-0.01 nm.

Hsiung, L. M.↗

NASA NTRS1992

Onset of dispersion in Nb microstrip transmission lines at submillimeter wave frequencies

We have measured the dispersion in phase velocity of a Nb-SiO(x)-Nb microstrip transmission line resonator over a frequency range from 50 GHz to 800 GHz. A submicron Nb/Al-AlO(x)/Nb Josephson junction was used as a voltage-controlled oscillator to excite the high order modes in the resonator. The same junction is used as a direct detector resulting in a series of step-like structures in the DC current-voltage characteristic at the position of each mode frequency. The transmission line is dispersionless up to about 500 GHz where the phase velocity begins to decrease. This is well below the gap frequency f(sub g) approx. equals 700 GHz. Results agree qualitatively with the expected theoretical behavior near f(sub g). This onset of dispersion and loss in Nb transmission lines will have a significant impact on the design of submillimeter wave RF circuits.

Javadi, H. H. S.↗

NASA NTRS1993

Effect of hydrogen exposure on a Cu-8 Cr-4 Nb alloy

The advanced regeneratively cooled rocket thrust chamber may require new materials to achieve long life and improved performance. Current materials such as NARloy-Z (Cu-3 wt. percent Ag-0.5 wt. percent Zr), while highly conductive, do not have sufficient high temperature strength and creep resistance to meet the projected needs of advanced rocket motors. A Cu-8 at. percent Cr-4 at. percent Nb (Cu-8 Cr-4 Nb) alloy has been identified as a promising material for this application. However, hydrogen embrittlement is a concern given the presence of high pressure, high temperature hydrogen in regeneratively cooled rocket motors. Thermodynamic analysis of the reaction between Cr-rich Cr2Nb and H2 showed that there is a possibility of reaction at temperatures up to 323 K in a 35 MPa H2 environment. Above 323 K the pressure necessary to achieve reaction rapidly increased beyond the range experienced in rocket motors. Tensile specimens exposed in 34.5 MPa H2 at room temperatures and during cycling to 705 C did not show any degradation of properties. No evidence of reaction was observed for Cr2Nb precipitate observed on the fracture surfaces. Based on these results the Cu-8 Cr-4 Nb alloy was judged to be sufficiently stable for use in rocket motors.

David L Ellis↗

NASA NTRS1994

Effects of thermomechanical processing on tensile and long-time creep behavior of Nb-1 percent Zr-0.1 percent C sheet

Effects of thermomechanical processing on the mechanical properties of Nb-1 wt. percent Zr-0.1 wt. percent C, a candidate alloy for use in advanced space power systems, were investigated. Sheet bars were cold rolled into 1-mm thick sheets following single, double, or triple extrusion operations at 1900 K. All the creep and tensile specimens were given a two-step heat treatment 1 hr at 1755 K + 2 hr 1475 K prior to testing. Tensile properties were determined at 300 as well as at 1350 K. Microhardness measurements were made on cold rolled, heat treated, and crept samples. Creep tests were carried out at 1350 K and 34.5 MPa for times of about 10,000 to 19,000 hr. The results show that the number of extrusions had some effects on both the microhardness and tensile properties. However, the long-time creep behavior of the samples were comparable, and all were found to have adequate properties to meet the design requirements of advanced power systems regardless of thermomechanical history. The results are discussed in correlation with processing and microstructure, and further compared to the results obtained from the testing of Nb-1 wt. percent Zr and Nb-1 wt. percent Zr-0.06 wt. percent C alloys.

Titran, Robert H.↗

NASA NTRS1996

High temperature coarsening of Cr2Nb precipitates in Cu-8 Cr-4 Nb alloy

A new high-temperature-strength, high-conductivity Cu-Cr-Nb alloy with a CrNb ratio of 2:1 was developed to achieve improved performance and durability. The Cu-8 Cr4 Nb alloy studied has demonstrated remarkable thermal and microstructural stability after long exposures at temperatures up to 0.98 T(sub m). This stability was mainly attributed to the slow coarsening kinetics of the Cr2Nb precipitates present in the alloy. At all temperatures, the microstructure consists of a bimodal and sometimes trimodal distribution of strengthening Cr2Nb precipitates, depending on precipitation condition, i.e. from liquid or solid solution, and cooling rates. These precipitates remain in the same size range, i.e. large precipitates of approximately I pm, and small precipitates less dm 300 nm, and effectively pin the grain boundaries thus retaining a fine grain size of 2.7 micro-m after 100 h at 1323 K. (A relatively small number of Cr-rich and Nb-rich particles were also present.) This grain boundary pinning and sluggish coarsening of Cr2Nb particles explain the retention of good mechanical properties after prolonged holding at very high temperatures, e.g., 75% of the original hardness after aging for 100 h at 1273 K. Application of LSW-based coarsening models indicated that the coarsening kinetics of the large precipitates are most likely governed by grain boundary diffsion and, to a lesser extent, volume diffusion mechanisms.

Anderson, Kenneth Reed↗