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Comparison of thermionic tungsten /110/ converter performances with niobium collectors and nickel collectors at various emitter, collector and cesium reservoir temperatures
This program demonstrated the feasibility of fabricating fiber-reinforced MMC (niobium matrix) turbine blades to net shape by chemical vapor infiltration (CVI). A controllable, repeatable niobium infiltration process was developed, and the kinetics of both deposition and infiltration were studied. Several continuous refractory fibers (Nicalon, Nextel 440, FP-Al2O3, HPZ, and tungsten mesh) were investigated as potential reinforcements for strengthening niobium. Thermodynamic and experimental evaluation indicated FP-Al2O3 and tungsten to be the most chemically compatible with niobium, while Nicalon, FP-Al2O3, and tungsten were found to be best with regard to reinforcing capability. Finally, a protective coating for iridium was found to provide substantial oxidation protection to the niobium blade matrix.
The field emission characteristics of niobium electrodes were compared to those of stainless steel electrodes using a DC high voltage field emission test apparatus. A total of eight electrodes were evaluated: two 304 stainless steel electrodes polished to mirror-like finish with diamond grit and six niobium electrodes (two single-crystal, two large-grain, and two fine-grain) that were chemically polished using a buffered-chemical acid solution. Upon the first application of high voltage, the best large-grain and single-crystal niobium electrodes performed better than the best stainless steel electrodes, exhibiting less field emission at comparable voltage and field strength. In all cases, field emission from electrodes (stainless steel and/or niobium) could be significantly reduced and sometimes completely eliminated, by introducing krypton gas into the vacuum chamber while the electrode was biased at high voltage. Of all the electrodes tested, a large-grain niobium electrode performed the best, exhibiting no measurable field emission (< 10 pA) at 225 kV with 20 mm cathode/anode gap, corresponding to a field strength of 18:7 MV/m.
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.
A study of the niobium hyperfine structure in single crystal calcium tungstate was made by the combination of the technique of electron paramagnetic resonance and electron nuclear double resonance (EPR/ENDOR). The microwave frequency was about 9.4 GHz and the radio frequency from 20MHz to 70 MHz. The rare earth ions Nd(3+), U(3+), or Tm(3+) were added as the charge compensator for Nb(5+). To create niobium paramagnetic centers, the sample was irradiated at 77 deg K with a 10 thousand curie Co-60 gamma source for 1 to 2 hours at a dose rate of 200 K rads per hour and then transferred quickly into the cavity. In a general direction of magnetic field, the spectra showed 4 sets of 10 main lines corresponding to 4 nonequivalent sites of niobium with I = 9/2. These 4 sets of lines coalesced into 2 sets of 10 in the ab-plane and into a single set of 10 along the c-axis. This symmetry suggested that the tungsten ions are substituted by the niobium ions in the crystal.
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.
Niobium pentoxide gels in the form of transparent monoliths and powder have been synthesized from the controlled hydrolysis and polycondensation of niobium pentaethoxide under different experimental conditions using various mole ratios of Nb(OC2H5)5:H2O:C2H5OH:HCl. Alcohol acted as the mutual solvent and HCl as the deflocculating agent. In the absence of HCl, precipitation of colloidal particles was encountered on the addition of any water to the alkoxide. The gels were subjected to various thermal treatments and characterized by differential thermal analysis, thermogravimetric analysis, x-ray diffraction, and infrared spectroscopy. After drying at 400 C, the gels were amorphous to x-rays. The amorphous powder crystallized into the low-temperature orthorhombic form of Nb2O5 at approximately 500 C, which transformed irreversibly into the high-temperature monoclinic alpha-Nb2O5 between 900 to 1000 C. The kinetics of crystallization of the amorphous niobium pentoxide have been investigated by non-isothermal differential scanning calorimetry. The crystallization activation energy was determined to be 399 kJ/mol.
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.
Niobium film superconductor carries high currents in strong magnetic fields. The thin niobium film is formed on an inert substrate through evaporation in a vacuum environment. Control of temperature and vacuum results in rejection of gaseous impurities so that the film is of a very high purity.
Study reveals the kinetics of niobium and tantalum with steam at elevated temperatures to determine the suitability of high melting metals for fabrication of equipment for temperature steam environments. Niobium obeyed linear kinetics from 1050 degrees to 1500 degrees C but tantalum followed a paralinear rate law.
Composite of fine niobium wires in copper is used to study the size and proximity effects of a superconductor in a normal matrix. The niobium rod was drawn to a 100 angstrom diameter wire on a copper tubing.
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.
The phase equilibrium relations of four systems were investigated in detail. These consisted of sodium and potassium antimonates with antimony oxide and tantalum and niobium oxide with rubidium oxide as far as the ratio 4Rb2O:llB2O5 (B=Nb, Ta). The ternary system NaSbO3-Sb2O4-NaF was investigated extensively to determine the actual composition of the body centered cubic sodium antimonate. Various other binary and ternary oxide systems involving alkali oxides were examined in lesser detail. The phases synthesized were screened by ion exchange methods to determine mobility of the mobility of the alkali ion within the niobium, tantalum or antimony oxide (fluoride) structural framework. Five structure types warranted further investigation; these structure types are (1) hexagonal tungsten bronze (HTB), (2) pyrochlore, (3) the hybrid HTB-pyrochlore hexagonal ordered phases, (4) body centered cubic antimonates and (5) 2K2O:3Nb2O5. Although all of these phases exhibit good ion exchange properties only the pyrochlore was prepared with Na(+) ions as an equilibrium phase and as a low porosity ceramic. Sb(+3) in the channel interferes with ionic conductivity in this case, although relatively good ionic conductivity was found for the metastable Na(+) ion exchanged analogs of RbTa2O5F and KTaWO6 pyrochlore phases.
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.
The creep resistance of tungsten fiber reinforced niobium metal-matrix composites was evaluated. The interface region between the fiber and matrix was characterized by microhardness and electron probe microanalysis measurements which indicated that its properties were between those of fiber and matrix. However, the measured properties of the composite exceeded those calculated by the rule of mixtures even when the interface zone was assumed to retain all the strength of the fiber. The composite structure appeared to enhance the strengths of both the fibers and the matrix above what they exhibited in stand-alone tests. The effect of fiber orientation and matrix alloy composition on the fiber/matrix interface were also evaluated. Small alloying additions of zirconium and tungsten to the niobium matrix affected the creep resistance of the composites only slightly. A decrease in the creep resistance of the composite with increasing zirconium content in the matrix was ascribed to an increase in the diffusion rate of the fiber/matrix interdiffusion reaction, and a slight increase in the creep resistance of the composite was observed with an addition of 9 w percent tungsten to the matrix. In addition, Kirkendall void formation was observed at the fiber/matrix interface; the void distribution differed depending on the fiber orientation relative to the stress axis.
Tungsten fiber reinforced niobium metal matrix composites were evaluated for use in space nuclear power conversion systems. The composite panels were fabricated using the arc-spray monotape technique at the NASA Lewis Research Center. The creep behavior of W/Nb composite material was determined at 1400 and 1500 K in vacuum over a wide range of applied loads. The time to reach 1 percent strain, the time to rupture, and the minimum creep rate were measured. The W/Nb composites exceeded the properties of monolithic niobium alloys significantly even when compared on a strength to density basis. The effect of fiber orientation on the creep strength also was evaluated. Kirkendall void formation was observed at the fiber/matrix interface; the void distribution differed depending on the fiber orientation relative to the stress axis. A relationship was found between the fiber orientation and the creep strength.
The microstructures of niobium aluminides produced by chill block melt spinning were compared to those of niobium aluminides produced by conventional casting. The rapidly solidified alloys were rapidly solidified by melt spinning in an argon atmosphere, and the melt-spun ribbons were examined by optical, X-ray, and TEM techniques. Microstructures were found to range from single-phase for Nb-75 at. pct Al (NbAl3) to two phase for Nb-46 at. pct Al (NbAl3 + Nb2Al). It was found that the melt spinning of Nb-aluminides produced finer grained microstructures than those produced in induction-melted ingots or in powders produced by the rotating electrode process. Ternary additions such as Cr, Ti, and Si tended to form intermetallic phases along the grain boundaries.
A novel technique is presented which should allow precise determination of the temperature dependence of the inductance, and hence of the penetration depth, of superconducting niobium thin-film structures. Four niobium thin-film stripline inductors are arranged in a bridge configuration, and inductance differences are measured using a potentiometric technique with a SQUID (superconducting quantum interference device) as the null detector. Numerical simulations of the stripline inductances are presented which allow the performance of the measurement technique to be evaluated. The prediction of the two-fluid model for the penetration-depth temperature dependence is given for reduced temperatures of 0.3 to 0.9. The experimental apparatus and its resolution and accuracy are discussed.