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Auto-vacuum cleaning technique was applied to titanium parts prior to welding. This provides oxide-free welding surfaces. Diffusion welding can be accomplished in as little as five minutes of hot pressing. Roll welding can be accomplished with only ten percent deformation.
Technique could be applied directly to loose powders as part of hot pressing process of forming them to any required shapes. This would eliminate initial extrusion step commonly applied to prealloyed powders, substantially reduce cost of forming operation, and result in optimum properties.
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.
Hot pressed silicon nitride was evaluated as a rolling element bearing material. The five-ball fatigue tester was used to test 12.7 mm (0.500 in.) diameter balls at a maximum Hertz stress of 800,000 psi at a race temperature of 130 F. The fatigue spalls in the silicon nitride resembled those in typical bearing steels. The ten-percent fatigue life of the silicon nitride balls was approximately one-eighth to one-fifth that of typical bearing steels (52100 and M-50). The load capacity of the silicon nitride was approximately one-third that of typical bearing steels. The load capacity of the silicon nitride was significantly higher than previously tested ceramic materials for rolling element bearings.
Crystal chemical principles and transport theory were used to predict structures and specific compounds which might find application as solid electrolytes in rechargeable high energy and high power density batteries operating at temperatures less than 200 C. More than twenty compounds were synthesized or obtained and screened by nuclear magnetic resonance and conductivity. Many were densified by sintering or hot pressing. Encouraging results were obtained for nine of these materials but none have yet been good ionic conductors at low temperature.
The deformation processes involved in the forging of refractory ceramic oxides were investigated. A combination of mechanical testing and forging was utilized to investigate both the flow and fracture processes involved. Deformation studies of very fine grain Al203 revealed an apparent transition in behavior, characterized by a shift in the strain rate sensitivity from 0.5 at low stresses to near unity at higher stresses. The behavior is indicative of a shift in control between two dependent mechanisms, one of which is indicated to be cation limited diffusional creep with significant boundary enhancement. The possible contributions of slip, indicated by crystallographic texture, interface control of the diffusional creep and inhomogeneous boundary sliding are also discussed. Additional experiments indicated an independence of deformation behavior on MgO doping and retained hot pressing impurities, at least for ultrafine grained material, and also an independence of test atmosphere.
Three approaches to the development of a high density scintillation glass were investigated: They include the increase of density of glass systems containing cerium - the only systems which were known to show scintillation, the testing of a novel silicate glass system containing significant concentrations of silver produced by ion exchange and never tested previously, and the hot pressing of a diphasic compact of low density scintillation glass with high density passive glass. In first two cases, while ultraviolet excited fluorescence was maintained in the glasses showing high density, scintillation response to high energy particles was not retained in the case of the cerium containing glasses or developed in the case of the silver containing glasses. In the case of the compacts, the extremely long path length caused by the multiple internal reflections which occur in such a body resulted in attenuation even with glasses of high specific transmission. It is not clear why the scintillation efficiency is not maintained in the higher density cerium containing glasses.
A screening, optimization, and evaluation program is reported of unidirectional carbon-aluminum composites. During the screening phase both large diameter monofilament and small diameter multifilament reinforcements were utilized to determine optimum precursor tape making and consolidation techniques. Difficulty was encountered in impregnating and consolidating the multifiber reinforcements. Large diameter monofilament reinforcement was found easier to fabricate into composites and was selected to carry into the optimization phase in which the hot pressing parameters were refined and the size of the fabricated panels was scaled up. After process optimization the mechanical properties of the carbon-aluminum composites were characterized in tension, stress-rupture and creep, mechanical fatigue, thermal fatigue, thermal aging, thermal expansion, and impact.
Pertinent mechanical properties of three high conductivity metals and alloys; namely, vacuum hot pressed grade S-200E beryllium, OFHC copper and beryllium-copper alloy no. 10 were determined. These materials were selected based on their possible use in rocket thrust chamber and nozzle hardware. They were procured in a form and condition similar to that which might be ordered for actual hardware fabrication. The mechanical properties measured include (1) tension and compression stress strain curves at constant strain rate (2) tensile and compressive creep, (3) tensile and compressive stress-relaxation behavior and (4) elastic properties. Tests were conducted over the temperature range of from 75 F to 1600 F. The resulting data is presented in both graphical and tabular form.
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.
Fabrication and microstructure control studies were conducted on SiC, Si3N and composites based on Si3N. Charpy mode impact testing to 2400 F established that Si3N4/Mo composites have excellent potential. Attempts to fabricate composites of Si3N4 with superalloys, both by hot pressing and infiltration were largely unsuccessful in comparison to using Mo, Re, and Ta which are less reactive. Modest improvements in impact strength were realized for monolithic Si3N4; however, SiC strengths increased by a factor of six and now equal values achieved for Si3N4. Correlations of impact strength with material properties are discussed. Reduced MgO densification aid additions to Si3N4 were found to decrease densification kinetics, increase final porosity, decrease room temperature bend strength, increase high temperature bend strength, and decrease bend stress rupture properties. The decrease in bend strength at high temperature for fine grain size SiC suggested that a slightly larger grain size material with a nearly constant strength-temperature relation may prove desirable in the creep and stress rupture mode.
Compression creep tests were investigated on various UC-based fuel materials having a variation in both density and composition. Specimens were prepared by casting and by hot pressing. Steady-state creep rates were measured under vacuum at 1400 to 1800 C in the stress range 500-4000 psi.
The thermal shock resistance of hafnia based composites containing graphite powder or tungsten fibers was investigated in terms of material properties which include thermal expansion, thermal conductivity, compressive fracture stress, modulus of elasticity, and phase stability in terms of the processing parameters of hot pressing pressure and/or density, degree of stabilization of the hafnia, and composition. All other parameters were held constant or assumed constant. The thermal shock resistance was directly proportional to the compressive fracture stress to modulus of elasticity ratio and was not affected appreciably by the small thermal expansion or thermal conductivity changes. This ratio was found to vary strongly with the composition and density such that the composites containing graphite had relatively poor thermal shock resistance, while the composites containing tungsten had superior thermal shock resistance.
Certain anions OH(-), F(-) and Gl(-) are shown to enhance grain growth in MgO. The magnitude of their effect decreases in the order in which the anions are listed and depends on their location (solid-solution, second phase) in the MgO lattice. As most anions exhibit relatively high vapor pressures at sintering temperatures, they retard densification and invariably promote residual porosity. The role of anions on grain growth rates was studied in relation to their effect on pore mobility and pore removal; the atomic process controlling the actual rates was determined from observed kinetics in conjunction with the microstructural features. With respect to controlling mechanisms, the effects of all anions are not the same. OH(-) and F(-) control behavior through creation of a defect structure and a grain boundary liquid phase while Cl(-) promotes matter transport within pores by evaporation-condensation. Studies on an additional anion, S to the minus 2nd power gave results which were no different from undoped MgO, possibly because of evaporative losses during hot pressing. Hence, the effect of sulphur is negligible or undetermined.
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.
A direct comparison of vacuum-melted, argon-atomized, hot-pressed, and extruded Unitemp C-300, an experimental, nickel-base superalloy, is made with as-cast and extruded material, with respect to mechanical properties and structural characteristics, utilizing the optimum thermomechanical processing variables previously established. Comparisons are also made with published mechanical properties of existing high temperature alloys in their temperature range of operation. These studies have established the exceptional versatility of this alloy for both high and low temperature applications and have shown that its strength characteristics significantly exceed those of the best currently available alloys on the market today.
Quenching was used to form compressive surface layers in hot-pressed silicon carbide. The presence of the compressive stresses was verified by slotted rod tests. The slotted rod tip deflection was retained at temperatures to at least 1380 C, showing that the stresses are not relieved immediately at elevated temperatures. The flexural strength and impact resistance of specimens quenched from moderate temperatures (2000 C) were increased. Frequently, specimens quenched from higher temperatures were weakened by thermal shock damage.
The first study area involved magnesium oxide and the role of anion impurities, while the second area was directed toward 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.