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Fabrication of cermets of uranium nitride and tungsten or molybdenum from mixed powders and from coated particles for nuclear fuel elements
Diffusion barrier research was focussed on lowering the chemical reactivity of amorphous thin films on silicon. An additional area of concern is the reaction with metal overlays such as aluminum, silver, and gold. Gold was included to allow for technology transfer to gallium arsenide PV cells. Amorphous tungsten nitride films have shown much promise. Stability to annealing temperatures of 700, 800, and 550 C were achieved for overlays of silver, gold, and aluminum, respectively. The lower results for aluminum were not surprising because there is an eutectic that can form at a lower temperature. It seems that titanium and zirconium will remove the nitrogen from a tungsten nitride amorphous film and render it unstable. Other variables of research interest were substrate bias and base pressure during sputtering.
Tungsten and titanium nitride films have long been grown by chemical vapor deposition (CVD) methods. However, there has been recent interest in low temperature growth using plasma enhanced CVD. For the present work, we focus on the radio frequency (BE) discharge characteristics of gas mixtures used in nitride deposition (for example, WF6 and ammonia). Because the radial variations for a standard 200 mm, parallel plate reactor are limited to a small zone near the edges of the electrodes, a 1-D (one-dimensional) analysis is considered. This model consists of a self-consistent, 3-D (three-dimensional) moment fluid simulation that solves the continuity, momentum, and energy equations for neutral and charged species. The results in terms of plasma structure, radical concentrations, and local deposition rate will be presented. We will also compare the 1-D results with those obtained from a 2-D hybrid plasma equipment model (HPEM) developed at the University of Illinois.
The Athena-plus team requires X-ray sensors with energy resolution of better than one part in 3,000 at 6 keV X-rays. While bismuth is an excellent material for high X-ray stopping power and low heat capacity (for large signal when an X-ray is stopped by the absorber), oxidation of the bismuth surface can lead to electron traps and other effects that degrade the energy resolution. Bismuth oxide reduction and nitride passivation techniques analogous to those used in indium passivation are being applied in a new technique. The technique will enable improved energy resolution and resistance to aging in bismuth-absorber-coupled X-ray sensors. Elemental bismuth is lithographically integrated into X-ray detector circuits. It encounters several steps where the Bi oxidizes. The technology discussed here will remove oxide from the surface of the Bi and replace it with nitridized surface. Removal of the native oxide and passivating to prevent the growth of the oxide will improve detector performance and insulate the detector against future degradation from oxide growth. Placing the Bi coated sensor in a vacuum system, a reduction chemistry in a plasma (nitrogen/hydrogen (N2/H2) + argon) is used to remove the oxide and promote nitridization of the cleaned Bi surface. Once passivated, the Bi will perform as a better X-ray thermalizer since energy will not be trapped in the bismuth oxides on the surface. A simple additional step, which can be added at various stages of the current fabrication process, can then be applied to encapsulate the Bi film. After plasma passivation, the Bi can be capped with a non-diffusive layer of metal or dielectric. A non-superconducting layer is required such as tungsten or tungsten nitride (WNx).
Plasma-sprayed oxide & vapor-deposited nitride protective coatings on tungsten
Two approaches were taken to make convenient spread sheet calculations of elastic constants from resonance data and the tables in ASTM C1259 and E1876: polynomials were fit to the tables; and an automated spread sheet interpolation routine was generated. To compare the approaches, the resonant frequencies of circular plates made of glass, hardened maraging steel, alpha silicon carbide, silicon nitride, tungsten carbide, tape cast NiO-YSZ, and zinc selenide were measured. The elastic constants, as calculated via the polynomials and linear interpolation of the tabular data in ASTM C1259 and E1876, were found comparable for engineering purposes, with the differences typically being less than 0.5 percent. Calculation of additional v values at t/R between 0 and 0.2 would allow better curve fits. This is not necessary for common engineering purposes, however, it might benefit the testing of emerging thin structures such as fuel cell electrolytes, gas conversion membranes, and coatings when Poisson s ratio is less than 0.15 and high precision is needed.
AMTEC cells are under development as power resources for future outer planetary robotic space missions, where they must operate for very long times.
The lifetime of three types of AMTEC electrodes is predicted from the rate of grain growth in the electrode.
Fuel loading requirements and resulting neutron energy spectrum after adding lithium nitride, hafnium, tantalum, and tungsten to molybdenum reflected critical assembly
High-purity nitride and carbide cermets were synthesized for compatability testing in liquid lithium. A process was developed for the preparation of high-purity hafnium nitride powder, which was subsequently blended with tungsten powder or tantalum nitride and tungsten powders and fabricated into 3 in diameter billets by uniaxial hot pressing. Specimens were then cut from the billets for compatability testing. Similar processing techniques were applied to produce hafnium carbide and zirconium carbide cermets for use in the testing program. All billets produced were characterized with respect to chemistry, structure, density, and strength properties.
The effect of tungsten and tungsten carbide contamination on the oxidation and cracking in air of yttria-doped silicon nitride ceramics is investigated. Silicon nitride powder containing 8 wt % Y2O3 was doped with 2 wt % W, 4 wt % W, 2 wt % WC or left undoped, and sintered in order to simulate contamination during milling, and specimens were exposed in air to 500, 750 and 1350 C for various lengths of time. Scanning electron and optical microscopy and X-ray diffraction of the specimens in the as-sintered state reveals that the addition of W or WC does not affect the phase relationships in the system, composed of alpha and beta Si3N4, melilite and an amorphous phase. Catastrophic oxidation is observed at 750 C in specimens containing 2 and 4 wt % W, accompanied by the disappearance of alpha Si3N4 and melilite from the structure. At 1350 C, the formation of a protective glassy oxide layer was observed on all specimens without catastrophic oxidation, and it is found that pre-oxidation at 1350 C also improved the oxidation resistance at 750 C of bars doped with 4 wt % W. It is suggested that tungsten contamination from WC grinding balls may be the major cause of the intermediate-temperature cracking and instability frequently observed in Si3N4-8Y2O3.
The feasibility of using uranium nitride for in-core thermionic applications was evaluated in electrically heated thermal gradient tests and in flat plate thermionic converters. These tests indicated that grain boundary penetration of uranium nitride into both tungsten and rhenium will occur under thermal gradient conditions. In the case of the tungsten thermionic converter, this led to grain boundary rupture of the emitter and almost total loss of electrical output from the converter. It appears that uranium nitride is unsuitable for thermionic applications at the 2000 K temperatures used in these tests.
The techniques used to fabricate cermet bearings for the fueled control drums of a liquid metal cooled reference-design reactor concept are presented. The bearings were designed for operation in lithium for as long as 5 years at temperatures to 1205 C. Two sets of bearings were fabricated from a hafnium carbide - 8-wt. % molybdenum - 2-wt. % niobium carbide cermet, and two sets were fabricated from a hafnium nitride - 10-wt. % tungsten cermet. Procedures were developed for synthesizing the material in high purity inert-atmosphere glove boxes to minimize oxygen content in order to enhance corrosion resistance. Techniques were developed for pressing cylindrical billets to conserve materials and to reduce machining requirements. Finishing was accomplished by a combination of diamond grinding, electrodischarge machining, and diamond lapping. Samples were characterized in respect to composition, impurity level, lattice parameter, microstructure and density.
This is the Monthly Letter Progress Report for the eighth month of a twelve month technical study directed toward the following objectives: A. Determining analytically and experimentally the feasibility and attractiveness of using free-standing pyrolytic graphite for a radiation cooled liquid rocket thrust chamber and exit nozzle for space application. B. Establishing through analysis and experimental demonstration, a set of design principles to facilitate the design of a reliable pyrolytic graphite thrust chamber assembly for a specific range of operating conditions. C. Demonstrate by means of test firings of complete thrust chamber assemblies, the validity of the design data and principles developed during the program. Preparations have been completed for test firing the two 100 lb. thrust Boron Pyralloy chambers at Marquardt during the first week in March 1962. These two chambers will first be static pressure checked with water to a pressure of 135 psig. The chambers will then be test fired with N204/N2H4-MMH propellants . Test samples of eleven different pyrolytic carbide and nitride materials have been ordered for high temperature oxidation tests and should be delivered by the end of March for evaluation in the plasma torch facility. The specific materials ordered in free- standing condition in thicknesses from 0.030 inch to 0.065 inch were as follows: (a) Pyrolytic graphite (on hand) (b) Pyrolytic graphite-boron alloy (on hand) (c) Pyrolytic graphite-tungsten alloy (d)Boron nitride (e) Titanium nitride (f) Silicon carbide (g) Titanium carbide (h) Zirconium carbide (i) Hafnium carbide (j) Niobium carbide (k) Tantalum carbide (l) High density (1 1-90) graphite (m) High density graphite (heat treated) These materials were ordered from Raytheon, HTM, and American Meta 1 Products . A summary of the available data on the oxidation rates of pyrolytic materials under slow air and rocket motor conditions is shown in Figure 1. High Temperature Materials, Inc. has been contacted relative to providing Pyrographite thrust chambers with extra-thick walls . They believe they can deliver chambers with substantially thicker walls than were possible a short time ago. Such a configuration, with acceptable residual stresses, would provide a longer firing life since it is ultimately limited by the oxidation rate of the chamber wall material. Stress and structural studies have continued. The analytical stress studies point out some of the problems associated with the experimental determination of the elastic constants of this highly anisotropic material. Further analysis may shed light on improved techniques for making these experimental determinations. The large potential weight saving available with the use of pyrolytic graphite as a thrust chamber wall material in a radiation cooled rocket motor has been calculated and is shown graphically in Figure 2. Figure A presents the program progress schedule and the actual expenditures as of 7 February 1962.
Tungsten-coated kernels of uranium nitride (UN) are a possible reactor fuel component for nuclear thermal propulsion. Hot hydrogen testing of such kernels (approx. 250μm diameter, coating thickness 5μm) has been performed at temperatures from 1800°C to 2300°C for 30min each, using depleted uranium nitride (dUN). In addition to direct observations and mass loss measurements, the samples were analyzed by XRD and SEM/EDS after each run. Decomposition of dUN and the formation of molten uranium happened at all temperatures tested with reaction rates increasing with temperature, despite the tungsten coating. At 2300°C, the kernels disintegrated and molten uranium seeped through the wall and bottom of the tungsten crucible employed. These hot hydrogen tests allowed to test the integrity of the tungsten coating and addressed the operating limits of the loose tungsten-coated dUN kernels. Improved results are expected upon consolidation of the tungsten-coated dUN kernels in a Mo-W alloy matrix.
A reliable isotope heat source simulator was designed for use in a Brayton power system. This simulator is composed of an electrically heated tungsten wire which is wound around a boron nitride core and enclosed in a graphite jacket. Simulator testing was performed at the expected operating temperature of the Brayton power system. Endurance testing for 5012 hours was followed by cycling the simulator temperature. The integrity of this simulator was maintained throughout testing. Alumina beads served as a diffusion barrier to prevent interaction between the tungsten heater and boron nitride core. The simulator was designed to maintain a surface temperature of 1311 to 1366 K (1900 to 2000 F) with a power input of approximately 400 watts. The design concept and the materials used in the simulator make possible man different geometries. This flexibility increases its potential use.
A mechanistically consistent model for indentation damage based on elastic failure at tensile or shear overloads, is proposed. The model accommodates arbitrary crack orientation, stress relaxation, reduction and recovery of stiffness due to crack opening and closure, and interfacial friction due to backward sliding of closed cracks. This elastic failure model was implemented by an axisymmetric finite element program which was used to simulate progressive damage in a silicon nitride plate indented by a tungsten carbide sphere. The predicted damage patterns and the permanent impression matched those observed experimentally. The validation of this elastic failure model shows that the plastic deformation postulated by others is not necessary to replicate the indentation damage of brittle structural ceramics.
Sialons were evaluated for application as high temperature electrical insulators in contact with molybdenum and tungsten components in hard vacuum applications. Both D.C. and variable frequency A.C. resistivity data indicate the sialons to have electrical resistivity similar to common oxide in the 1000 C or higher range. Metallographic evaluations indicate good bonding of the type 15R ALN polytype to molybdenum and tungsten. The beta prime or modified silicon nitride phase was unacceptable in terms of vacuum stability. Additives effect on electrical resistivity. Similar resistivity decreases were produced by additions of molybdenum or tungsten to form cermets. The use of hot pressing at 1800 C with ALN, Al2 O3 and Si3N4 starting powders produced a better product than did a combination of SiO2 and AIN staring powders. It was indicated that sialons will be suitable insulators in the 1600K range in contact with molybdenum or tungsten if they are produced as a pure ceramic and subsequently bonded to the metal components at temperatures in the 1600K range.