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Strengthening of chemically consolidated zirconia with tungsten fibers, graphite fibers, sapphire whiskers, and silicon carbide whiskers is investigated. Addition of silicon carbide whiskers gives the highest increase in strength of zirconia at room and elevated temperatures. Prestressing with tungsten cables increases tensile strength and ductility
An evaluation is presented of silicon carbide, zirconium diboride, and iridium-coated graphite as materials for construction of furnace cores which could operate under highly oxidizing conditions at temperatures of approximately 2,200 C in the presence of molten aluminum oxide. It was found that silicon carbide and zirconium diboride could not withstand oxidizing atmospheres in the presence of aluminum oxide at temperature 2,200 C. However, graphite furnace cores coated with iridium were found to be useful furnace cores at 2,200 C in an oxidizing atmosphere for reasonably extended periods of time.
By means of transmission electron microscopy and electron diffraction, evidence has been obtained for the existence of long range carbon atom ordering in single-crystal niobium carbide that has a carbon-to-metal ratio close to the integral composition Nb6C5. The ordering, which gives rise to superlattice and domain structures similar to those observed in V6C5, appears, however, only in samples that have been cooled slowly through the order-disorder temperature of 1025 C. In TaC of similar composition, the ordering, although present, remains very imperfect even after the crystals are subjected to the same thermal treatment. The results are interpreted in terms of the electronic structure of the transition metal carbides as it is currently understood, and their relevance to the mechanical properties of NbC and TaC are discussed.
The effect of microstructures of tungsten cladding on the transport rates of carbide fuel components was studied at 2073 K. hyperstoichiometric 90UC-10ZrC containing 4 wt% tungsten was clad with six types of tungsten material of 40 mil thickness. Screening tests of 1000 hours were carried out, and then selected samples were subjected to long-term tests up to 10,000 hours. The results indicate that the microstructures strongly affect the transport rates of carbide fuel components. The conditions for preparing (110) oriented cylindrical chloride tungsten emitters of high vacuum work functions were also investigated. Specimen sets were deposited on fluoride tungsten substrates for evaluating the effects of various deposition parameters on the degree and uniformity of the (110) preferred orientation and the vacuum work function. Long-term tests showed that the high vacuum work function of a cylindrical emitter was stable and the chloride tungsten to fluoride tungsten bond remained in excellent shape after 4850 hours at 2073 K.
Fuel-cladding systems capable of maintaining stable dimension and electron emission characteristics at high temperatures under irradiation are essential to the successful operation of nuclear thermionic power sources. Studies regarding two possible systems, involving tungsten clad uranium carbide and uranium oxide, are considered. Out-of-pile developmental efforts and the in-pile evaluation results for the two systems are described. Prototypical emitters have been tested for 8000 hours for the carbide system and 4000 hours for the oxide system.
The behavior and properties of the refractory carbides, nitrides, and borides are being investigated by NASA as part of its research aimed at developing superior heat resistant materials for aerospace applications. Fundamental studies on the electronic and defect structures of the carbides indicate that there is promise for improving the strength and ductility of these materials. Studies of the zirconium-carbon-oxygen system show that zirconium oxycarbides of different compositions and lattice parameters can be formed between 1500 and 1900 C and are stable below 1500 C. More applied studies show that hot working generally improves the microstructure and therefore the strength of TiC and NbC. Sintering studies on UN indicate that very high densities can be achieved. Hot pressing of cermets of HfN and HfC produces good mechanical properties for high temperature bearing applications.
An exploratory evaluation of ceramics for automobile thermal reactors was conducted. Potential ceramic materials were evaluated in several reactor designs using both engine dynamometer and vehicle road tests. Silicon carbide contained in a corrugated metal support structure exhibited the best performance lasting over 800 hours in engine dynamometer tests and over 15,000 miles (24,200 km) of vehicle road tests. Reactors containing glass-ceramic components did not perform as well as silicon carbide. But the glass-ceramics still offer good potential for reactor use. The results of this study are considered to be a reasonable demonstration of the potential use of ceramics in thermal reactors.
Compressive surface layers were formed on hot-pressed silicon carbide and nitride. The objective of these treatments was to improve the impact resistance of these materials at 1590 K (2400 F). Quenching was used to form compressive surface layers on silicon carbide. The presence of the compressive stresses was demonstrated by slotted rod tests. Compressive stresses were retained at elevated temperatures. Improvements in impact resistance at 1590 K (2400 F) and flexural strength at room temperature were achieved using cylindrical rods 3.3 mm (0.13 in.) in diameter. Carburizing treatments were used to form the surface layers on silicon nitride. In a few cases using rectangular bars improvements in impact resistance at 1590 K (2400 F) were observed.
Superalloys containing chromium showed decreasing fretting damage with increasing temperature of 816 C. This trend was related to the ability of the alloys to generate self-protecting oxide films. The damage at 816 C was one-third to one-tenth of that at 23 C. Osmium, chromium, and chromium carbide platings were fretted at 23 and 450 C. Osmium was extremely protective at 23 C but oxidized excessively at 450 C. Chromium and chromium carbide gave about the same protection at 450 C as the oxide films that formed on the superalloys. High graphite and low graphite carbons were fretted at 23 and 327 C. High graphite carbon was superior at 327 C, but low graphite carbon was the best material examined at 23 C.
Several fast-spectrum space power reactor concepts that use boron carbide control devices were examined to determine the neutronic feasibility of the designs. The designs considered were (1) a 199-fuel-pin, 12-poison-reflector-control-drum reactor; (2) a 232-fuel-pin reactor with 12 reflector drums and three in-core control rods; (3) a 337-fuel-pin design with 12 incore control rods; and a 181-fuel-pin design with six drums closely coupled to the core to increase reactivity per drum. Adequate reactivity control and excess reactivity could be obtained for each concept, and the goals of 50,000 hours at 2.17 thermal megawatts with a lithium-7 coolant outlet temperature of 1222 K could be met without exceeding the 1-percent-clad-creep criterion. Heating rates in the boron carbide were calculated, but a heat transfer analysis was not done.
Oxidation experiments were conducted with several experimental mechanical carbons at 650 C in air flowing at 28 cu cm/sec (STP). Experiments indicate that boron carbide addition and zinc phosphate treatment definitely improved oxidation resistance. Impregnation with coal tar pitch before final graphitization had some beneficial effect on oxidation resistance and it markedly improved flexure strength and hardness. Graphitization temperature alone did not affect oxidation resistance, but with enough added boron carbide the oxidation resistance was increased although the hardness greatly decreased.
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.
Extraction, hydrolysis, and crushing procedures have been useful in discovering some of the carbon compounds in lunar samples from the Apollo 11 and 12 missions. The nonaqueous solvent system used mostly in lunar sample work has been benzene:methanol. Two methods of extraction have been sonication and Soxhlet extraction, sonication appearing to be the preferred method. Extraction of lunar samples with water and acid hydrolysis of the water extract has proved to be the best method in the search for amino acids or their precursors. Direct acid hydrolysis of lunar samples provided evidence for the presence of carbides or carbide-like materials in lunar surface samples. Hydrolysis of lunar samples with DF, DC1, and NaOD has shown that methane and ethane are indigenous to the moon.
The results obtained in an exploratory evaluation of ceramics for automobile thermal reactors are summarized. Candidate ceramic materials were evaluated in several reactor designs by using both engine-dynamometer and vehicle road tests. Silicon carbide contained in a corrugated-metal support structure exhibited the best performance, lasting 1100 hr in engine-dynamometer tests and more than 38,600 km (24000 miles) in vehicle road tests. Although reactors containing glass-ceramic components did not perform as well as those containing silicon carbide, the glass-ceramics still offer good potential for reactor use with improved reactor designs.
Various properties of ceramic materials were investigated. Magnesium oxide and the role of anion impurities were investigated together with the slow crack growth in silicon nitride-silicon carbide ceramics. The oxide program involved development of fabrication techniques for anion doped materials and evaluation of the role of these anions in the hot pressing response, grain boundary diffusion of nickel doped material, grain boundary microhardness, and grain growth. The carbide-nitride work employed commercial materials and the research involved evaluation of a recently reported technique for study of slow crack growth and the development of data for these commercial materials.
Silicon nitride and silicon carbide ceramics were treated to form compressive surface layers. On the silicon carbide, quenching and thermal exposure treatments were used, and on the silicon nitride, quenching, carburizing, and a combination of quenching and carburizing were used. In some cases substantial improvements in impact resistance and/or flexural strength were observed. The presence of compressive surface stresses was demonstrated by slotted rod tests.
Evaluation of tantalum carbide-tungsten fiber composites has been completed as far as weight percent carbon additions and weight percent additions of tungsten fiber. Extensive studies were undertaken concerning Young's Modulus and fracture strength of this material. Also, in-depth analysis of the embrittling effects of the extra carbon additions on the tungsten fibers has been completed. The complete fabrication procedure for the tantalum carbide-tungsten fiber composites with extra carbon additions is given. Microprobe and metallographic studies showed the effect of extra carbon on the tungsten fibers, and evaluation of the thermal shock parameter fracture strength/Young's Modulus is included.
Studies were conducted to determine the friction and wear properties of experimental carbon-graphites. Hemispherically tipped carbon-graphite rider specimens were tested in sliding contact with rotating Inconel X-750 disks in air. A surface speed of 1.33 m/sec, a load of 500 g, and a specimen temperature of 650 C were used. Results indicate: (1) hardness is not a major factor in determining friction and wear under the conditions of these studies. (2) Friction and wear as low as or lower than those observed for a good commercial seal material were attained with some of the experimental materials studied. (3) The inclusion of boron carbide (as an oxidation inhibitor) has a strong influence on wear rate. (4) Phosphate treatment reduces the friction coefficient when boron carbide is not present in the base material.