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At least 649 records · Page 36
All sourcesNASA NTRSDOE OSTI
DOE OSTI2024

Radiological Characterization of Uranium Decay Products in LEU U-10Mo Before and After Heat Treatment

Fuel for the U.S. high-performance research reactor fleet is undergoing significant development as the United States moves away from using highly enriched uranium dispersion fuels. The proposed fuel is a high-density, low-enriched uranium (LEU, 19.75 wt% U 235) alloyed with ten weight percent molybdenum fuel (known as LEU U 10Mo). The LEU U 10Mo fuel samples studied in this report were made by down-blending highly enriched uranium with a master alloy, which is cast from molybdenum rods and depleted uranium, via vacuum induction melting and then casting.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2026

Influence of Powder Characteristics and Processing Methods on Creep Performance of Powder Metallurgy Hot Isostatic Pressed SS316

The U.S. nuclear energy expansion goals are driving the demand for manufacturing routes that can rapidly produce large, complex, near net shape components. Powder metallurgy hot isostatic pressing (PM HIP) is an advanced manufacturing technique that can be economically scaled-up, while alleviating the supply chain challenges that forging and casting face in terms of cost and lead time constraints. This makes PM-HIP a viable technology to aid and accelerate large-scale part manufacturing for nuclear applications. However, large-scale qualification and deployment of this technology require a thorough understanding of the influence of powder feedstock quality, powder handling history, hot isostatic pressing (HIP) parameters, and subsequent heat treatment on microstructural evolution and elevated temperature mechanical performance. The present work focusses on 316 austenitic stainless steel (SS316) which is most commonly used in high temperature environments for nuclear applications Results from this study show that PM HIPed SS316 meets ASME tensile requirements at room temperature and at elevated temperature. However, creep performance of PM-HIPed SS316 remains inferior to its wrought counterpart, demonstrating that tensile performance alone is not a reliable metric for long duration high temperature integrity. Further, this report delineates powder derived microstructural features that govern creep damage, with key evidences pointing to “microstructural inheritance” from gas atomized powder feedstocks. Commercial SS316 powders of varying chemical compositions and recycling histories were studies, and the results showed large differences in elemental segregation, oxide surface layers and secondary phase distributions. Multi-scale characterization revealed segregation of chromium, molybdenum, manganese and silicon at the boundaries and the precipitation of manganese-, silicon-, and molybdenum-oxides. During HIP consolidation, these surface oxides transform into decorated prior particle boundaries (PPBs) and grain boundary inclusions that persist through conventional post-HIP solution annealing treatment. The retained oxides in post-HIP microstructures were found to influence grain growth, precipitation behavior, and ultimately creep cavitation and fracture. Such post-HIP heat treatments are therefore limited by a complex trade-off between grain growth, and oxide coarsening which aggravate creep damage by acting as nucleation sites for cavities. The objective of this work is to establish an integrated processing–structure–property framework for PM-HIP 316 stainless steel by investigating the influence of powder feedstock characteristics in pre- and post-HIP processing as well as to understand the significance of post-HIP heat treatment on microstructural evolution and creep properties. The results from this report emphasize the significance of powder feedstock integrity in improving creep performance of PM-HIPed SS316, by highlight the effect of rapid solidification, elemental segregation, oxide formation and powder recycling on microstructural defect inheritance following HIP consolidation. Rather than considering HIP processing, solution annealing, and mechanical performance independently, this report treats powder production, HIP consolidation, post-HIP thermal processing, and creep deformation as interconnected stages within a continuous metallurgical process. The resulting framework will provide a scientific basis for developing feedstock engineering strategies capable of improving long-term reliability of PM-HIP stainless steels and accelerating their qualification for advanced nuclear applications.

Ajjarapu, Pavan [Oak Ridge National Laboratory (OR↗
DOE OSTI2025

Steam-Assisted Ammonolysis of MoO2 as a Synthetic Pathway to Oxygenated δ-MoN

A common route for the synthesis of molybdenum nitrides is through the temperature-programmed reaction of molybdenum oxides with NH3, or ammonolysis. In this work, the role of precursor phase, gas phase chemistry (impact of H2O), and temperature profile on the reaction outcome (700 °C) was examined, which resulted in varying amounts of MoO2, H2MoO5, and the nitride phases—cubic γ (nominally Mo2N) and hexagonal δ (nominally MoN). The phase fraction of the δ phase increased with precursor in the sequence MoO2 > MoO3 > H2MoO5. Steam in the reaction gas also favored the production of δ over γ, but with too much steam, MoO2 was obtained in the product. Synthesis conditions for obtaining nearly phase-pure δ were identified: MoO2 as the precursor, 2% H2O in the gas stream, and a moderate heating rate (3 °C/min). In situ X-ray diffraction provided insights into the reaction pathway. Extensive physico-chemical analysis of the δ phase, including synchrotron X-ray and neutron diffraction, electron microscopy, thermogravimetric analysis, X-ray photoelectron spectroscopy, and prompt gamma activation analysis, revealed its stoichiometry to be MoO0.108(8)N0.892(8)H0.012(5), indicating non-trivial oxygen incorporation. The presence of N/O ordering and an impurity phase Mo5N6 were also revealed, detectable only by neutron diffraction. Notably, a computationally predicted MoON phase (doi: 10.1103/PhysRevLett.123.236402), of interest due to its potential to display a metal-insulator transition, did not appear under any reaction condition examined.

Pandey, Shobhit↗
NASA NTRS1972

Metallic transfer between metals in sliding contact examined by auger emission spectroscopy

Metallic transfer between polycrystalline metals in sliding contact was examined. Hemispherical riders of iron, nickel, and cobalt were slid on tungsten, tantalum, niobium, and molybdenum disks in ultrahigh vacuum. Auger emission spectroscopy was used to monitor the elemental composition of the disk surfaces. Iron, nickel, and cobalt transferred to tungsten, whereas only cobalt transferred to tantalum, niobium, and molybdenum. The results of this investigation are discussed in terms of the cohesive energy and strain hardening characteristics of the specimen materials.

Pepper, S. V.↗
NASA NTRS1975

Structure and elevated temperature properties of carbon-free ferritic alloys strengthened by a Laves phase

A Laves phase, Fe2Ta, was utilized to obtain good elevated temperature properties in a carbon-free iron alloy containing 1 at. pct Ta and 7 at. pct Cr. Room temperature embrittlement resulting from the precipitation of the Laves phase at grain boundaries was overcome by spheroidizing the precipitate. This was accomplished by thermally cycling the alloys through the alpha to gamma transformation. The short-time yield strength of the alloys decreased very slowly with increase in test temperature up to 600 C, but above this temperature, the strength decreased rapidly. Results of constant load creep and stress rupture tests conducted at several temperatures and stresses indicated that the rupture and creep strengths of spheroidized 1 Ta-7 Cr alloy were higher than those of several commercial steels containing chromium and/or molybdenum carbides but lower than those of steels containing substantial amounts of tungsten and vanadium. When molybdenum was added to the base Fe-Ta-Cr alloy, the rupture and creep strengths were considerably increased.

Bhandarkar, M. D.↗
NASA NTRS1977

Susceptibility to hot corrosion of four nickel-base superalloys, NASA-TRW VIA, B-1900, 713C and IN-738

The susceptibility to hot corrosion of four nickel-base, cast superalloys has been studied at 900 and 1000 C. The test consisted of coating alloy samples with known amounts of Na2SO4 and oxidizing the coated samples isothermally in 1 atmosphere of slowly flowing oxygen, the weight-gain being monitored on a sensitive recording microbalance. Susceptibility to hot corrosion decreased in the order of decreasing molybdenum content of the alloys. Preoxidation of samples before hot-corrosion testing markedly increased the induction period observed prior to the inception of hot corrosion for all alloys tested. X-ray diffraction analyses of the oxide scales were made. All samples that underwent hot corrosion showed the presence of a (Ni,Co)MoO4 layer near the alloy-oxide interface. Several specimens displayed resistance to hot corrosion and these showed NaTaO3 as a prominent feature in their oxide scale. Our results may be interpreted as indicating that molybdenum in an alloy is detrimental, with respect to hot corrosion, while tantalum is beneficial.

Stearns, C. A.↗
NASA NTRS1977

Friction and wear properties of three hard refractory coatings applied by radiofrequency sputtering

The adherence, friction, and wear properties of thin hard refractory compound coatings applied to 440C bearing steel by radiofrequency sputtering were investigated. Friction and wear tests were done with nonconforming pin on disk specimens. The compounds examined were chromium carbide, molybdenum silicide, and titanium carbide. The adherence, friction, and wear were markedly improved by the application of a bias voltage to the bearing steel substrate during coating deposition. Analysis by X-ray photoelectron spectroscopy indicated that the improvement may be due to a reduction in impurities in bias deposited coatings. A fivefold reduction in oxygen concentration in MoSi2 coating by biasing was noted. Chromium carbide was not effective as an antiwear coating. Molybdenum silicide provided some reduction in both friction and wear. Titanium carbide exhibited excellent friction and antiwear properties at light loads. Plastic flow and transfer of the coating material onto the pin specimen appears to be important in achieving low friction and wear.

Brainard, W. A.↗
NASA NTRS1978

Modified chemiluminescent NO analyzer accurately measures NOX

Installation of molybdenum nitric oxide (NO)-to-higher oxides of nitrogen (NOx) converter in chemiluminescent gas analyzer and use of air purge allow accurate measurements of NOx in exhaust gases containing as much as thirty percent carbon monoxide (CO). Measurements using conventional analyzer are highly inaccurate for NOx if as little as five percent CO is present. In modified analyzer, molybdenum has high tolerance to CO, and air purge substantially quenches NOx destruction. In test, modified chemiluminescent analyzer accurately measured NO and NOx concentrations for over 4 months with no denegration in performance.

Summers, R. L.↗
NASA NTRS1979

Recent progress in hybrid mode thermionic converter development

Thermionic research has been conducted to investigate a hybrid-mode thermionic converter as a candidate for reducing the barrier index. The hybrid-mode thermionic converter is designed to operate in a combination ignited mode and unignited mode by using a series of parallel grooves in the emitter. The emitter material is molybdenum and the non-grooved land area is thinly coated with rhenium metal. When the emitter is exposed to cesium vapor, as it is during the converter operation, the rhenium-coated land area achieves a lower work function than the grooved molybdenum surface by as much as 0.5 eV. The low work function land area provides a major portion of electron emission, and the high work function grooved area provides cesium ions required for efficient transport of electrons generated in adjacent land areas to the collector. Experimental results obtained from two different converters and a numerical analysis of converter characteristics are presented in this paper.

Shimada, K.↗
NASA NTRS1979

Low cost cylindrical converter for measuring lead efficiency

A low cost cylindrical thermionic converter has been designed, fabricated, and tested for use in a NASA-JPL program to directly measure converter lead efficiencies using various electrode materials and surfaces. Efficiency measurements are made using input emitter heater power, output power at the leads, and calculated values of the parasitic losses that would not be present in the application configuration. This information can be used to predict the performance characteristics of the advanced converters currently under development. A series of five converters has been tested. Both structured and smooth molybdenum collectors have been used. Emitters included smooth molybdenum, smooth rhenium, and microstructured rhenium. Cesium pressure families of current-voltage curves are presented for emitter temperatures of 1600, 1700, and 1800 K, along with measured efficiencies as a function of converter current densities for each temperature.

Hatch, G. L.↗
NASA NTRS1980

Effects of impurities in coal-derived liquids on accelerated hot corrosion of superalloys

A Mach 0.3 burner rig was used to determine the effects of potential coal derived liquid fuel impurity combustion of products on hot corrosion in IN-100, IN-792, IN_738, U-700, Mar M-509, and 304 stainless steel. The impurities, added as aqueous solutions to the combustor, were salts of sodium, potassium, vanadium, molybdenum, tungsten, phosphorus, and lead. Extent of attack was determined by metal consumption and compared to the effects of sodium alone. Vanadium, molybdenum, tungsten, phosphorous, and lead in combination with sodium all resulted in increased attack as compared with sodium alone at some temperatures, apparently due in large part to the extension of the formation of liquid deposits. Varying the sodium-potassium ratio had little effect for ratios less than 1:3 for which reduced, but measurable, attack was observed.

Deadmore, D. L.↗
NASA NTRS1979

Efficient solar cells by space processing

Thin films of electron beam evaporated silicon were deposited on molybdenum, tantalum, tungsten and molybdenum disilicide under ultrahigh vacuum conditions. Mass spectra from a quadrapole residual gas analyzer were used to determine the partial pressure of 13 residual gases during each processing step. Surface contamination and interdiffusion were monitored by in situ Auger electron spectrometry. The presence of phosphorus in the silicon was responsible for attaining elevated temperatures with silicide formations. Heteroepitaxial silicon growth was sensitive to the presence of oxygen during deposition, the rate and length of deposition as well as the substrate orientation.

Schmidt, F. A.↗
NASA NTRS1980

Ion and advanced electric thruster research

A phenomenological model of the orificed, hollow cathode based on the field enhanced, thermionic mechanism of electron emission is presented. High frequency oscillations associated with the orificed, hollow cathode are shown to be a consequence of current flow through the cathode orifice. A procedure for Langmuir probing of the hollow cathode discharge and analyzing the resulting probe characteristics is discussed. The results of sputter yield measurements made for molybdenum, tantalum, type 304 stainless steel and copper surfaces being bombarded by low energy argon or mercury ions are also given. The effects of nitrogen and alternated copper layers on the sputter yields of molybdenum, tantalum and 304 stainless steel are also discussed. A dynamic model of electrothermal rocket and ramjet thrusters is developed. The gross performance of these devices is compared to that of an electromagnetic gun for the case of a high acceleration, Earth launch mission. The theoretical performance of electrothermal rockets and ramjets is shown to be comparable to that of the electromagnetic gun.

Wilbur, P. J.↗
NASA NTRS1981

Thermal fatigue behavior of H-13 die steel for aluminum die casting with various ion sputtered coatings

Sputtered coatings of Mo, W, Pt, Ag, Au, Co, Cr, Ni, Ag + Cu, Mo + Pt, Si3N4, A1N, Cr3C2, Ta5Si3, and ZrO2 were applied to a 2-inch-square, 7-inch-long thermal fatigue test specimen which was then internally water cooled and alternately immersed in molten aluminum and cooled in air. After 15,000 cycles the thermal fatigue cracks at the specimen corners were measured. Results indicate that a significant improvement in thermal fatigue resistance was obtained with platinum, molybdenum, and tungsten coatings. Metallographic examination indicates that the improvement in thermal fatigue resistance resulted from protection of the surface of the die steel from oxidation. The high yield strength and ductility of molybdenum and tungsten contributed to the better thermal fatigue resistance.

Nieh, C. Y.↗
NASA NTRS1982

Holographic fabrication of gratings in metal substrates

A program for investigating the grain enlargement resulting from the laser recrystallization of a thin gallium arsenide film on a patterned substrate, a technique known as graphoepitaxy was evaluated. More specifically, the effects of recrystallizing an uncapped gallium arsenide film using a continuous wave neodymium YAG laser operating at 1.06 microns were studied. In an effort to minimize arsenic loss from the film, the specimens were held in an arsine atmosphere during recrystallization. Two methods for fabricating patterned substrates were developed, one using reactive ion etching of a molybdenum film on both sapphire and silicon substates and another by preferential wet etching of a silicon substrate onto which a film of molybdenum was subsequently deposited.

Fletcher, R. M.↗
NASA NTRS1984

Orbiting dynamic compression laboratory

In order to examine the feasibility of carrying out dynamic compression experiments on a space station, the possibility of using explosive gun launchers is studied. The question of whether powders of a refractory metal (molybdenum) and a metallic glass could be well considered by dynamic compression is examined. In both cases extremely good bonds are obtained between grains of metal and metallic glass at 180 and 80 kb, respectively. When the oxide surface is reduced and the dynamic consolidation is carried out in vacuum, in the case of molybdenum, tensile tests of the recovered samples demonstrated beneficial ultimate tensile strengths.

Ahrens, T. J.↗
NASA NTRS1985

Iron rich low cost superalloys

An iron-rich low-cost superalloy was developed. The alloy, when processed by conventional chill casting, has physical and mechanical properties that compare favorably with existing nickel and cobalt based superalloys while containing significantly lower amounts of strategic elements. Studies were also made on the properties of Cr(20)-Mn(10)-C(3.4)-Fe(bal.), a eutectic alloy processed by chill casting and directional solidification which produced an aligned microstructure consisting of M7C3 fibers in a gamma-Fe matrix. Thermal expansion of the M7C3 (M = Fe, Cr, Mn) carbide lattice was measured up to 800 C and found to be highly anisotropic, with the a-axis being the predominant mode of expansion. Repetitive impact sliding wear experiments performed with the Fe rich eutectic alloy showed that the directionally solidified microstructure greatly improved the alloy's wear resistance as compared to the chill cast microstructure and conventional nickel base superalloys. Studies on the molybdenum cementite phase prove that the crystal structure of the xi phase is not orthorhombic. The crystal structure of the xi phase is made up of octahedra building elements consisting of four Mo and two Fe atoms and trigonal prisms consisting of four Fe and two Mo atoms. The voids are occupied by carbon atoms. The previous chemical formula for the molybdenum cementite MoFe2C is now clearly seen to be Mo12Fe22C10.

Wayne, S. F.↗