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The presence of copper promotes a more rapid approach to the steady stete operating condition and results in a more consistent reactor effluent composition. The average kinetic and equilibrium yield are unchanged. Incoloy has been identified as the preferred choice of material of construction for the hydrogenation reactor although certain metallurgical changes were noted in samples exposed to the H2/HCl atmosphere at 500 C which indicate the need for more testing.
Development of inside diameter slicing technology to significantly increase the number of useable slices per inch of crystal over industry practice is discussed. The required reduction of both blade and slice thickness is to be accomplished by a combination of three key elements of slicing technology: (1) ingot rotation with minimum exposed blade area; (2) dynamic cutting edge control; and (3) the use of prefabricated insert blades. Design modifications on a slicing saw with microprocessor controls and hardware fabrication to complete this conversion were initiated. Several runs were conducted on the engineering saw incorporating the method of ingot rotation. Ingots with diameters up to six inches were sliced successfully on a production saw.
The results of the free space reactor experimental work are summarized. Overall, the objectives were achieved and the unit can be confidently scaled to the EPSDU size based on the experimental work and supporting theoretical analyses. The piping and instrumentation of the fluidized bed reactor was completed.
Modifications to a 16 inch STC automated saw included: a programmable feed system; a crystal rotating system; and a STC dynatrack blade boring and control system. By controlling the plating operation and by grinding the cutting edge, 16 inch I.D. blades were produced with a cutting edge thickness of .22 mm. Crystal rotation mechanism was used to slice 100 mm diameter crystals with a 16 inch blade down to a thickness of .20 mm. Cutting rates with crystal rotation were generally slower than with standard plunge I.D. slicing techniques. Using programmed feeds and programmed rotation, maximum cutting rates were from 0.3 to 1.0 inches per minute.
Conventional and microfocus X-radiographic techniques were compared to determine relative detectability limits for voids in green and sintered SiC and Si3N4. The relative sensitivity of the techniques was evaluated by comparing their ability to detect voids that were artificially introduced by a seeding process. For projection microfocus radiography the sensitivity of void detection at a 90/95 probability of detection/confidence level is 1.5% of specimen thickness in sintered SiC and Si3N4. For conventional contact radiography the sensitivity is 2.5% of specimen thickness. It appears that microfocus projection radiography is preferable to conventional contact radiography in cases where increased sensitivity is required and where the additional complexity of the technique can be tolerated.
This study examines the effect of modifications of the chemical structure of the monomers on the properties of the polymeric precursor and and ceramic fibers. A group of silaneamines, R'-Si (NH-R) sub 3, taken from the series where R' is methyl or phenyl and R is n-propyl, n-butyl, phenyl or allyl, are converted to polycarbosilazanes by heating in excess of 500 C. Resins obtained from this polymerization are characterized by NMR and IR spectroscopy and GPC. Each resin is tested for fiber-forming properties. Resin samples and fibers are hydrolytically cured. Thermogravimetric analyses are conducted on the cured resins to compare the relative thermal stability and examine the pyrolysis process. Cured fibers are tested for tensil strength.
Conventional and microfocus X-radiographic techniques were compared to determine relative detectability limits for voids in green and sintered SiC and Si3N4. The relative sensitivity of the techniques was evaluated by comparing their ability to detect voids that were artificially introduced by a seeding process. For projection microfocus radiography the sensitivity of void detection at a 90/95 probability of detection/confidence level is 1.5 percent of specimen thickness in sintered SiC and Si3N4. For conventional contact radiography the sensitivity is 2.5 percent of specimen thickness. It appears that microfocus projection radiography is preferable to conventional contact radiography in cases where increased sensitivity is required and where the additional complexity of the technique can be tolerated.
The influence on density and strength of pressureless sintering in vacuum and argon environments has been evaluated with injection molded SiC materials. Main effects and two factor interactions of sintering (cycle variables temperature, time, heating rate, and atmosphere) were assessed. An improved understanding of the influence of the processing flaws and sintering conditions has been obtained. Strength and density have improved from a baseline level of 299 MPa (43.3 Ksi) and 94 pct of theoretical density to values greater than 483 MPa (70 Ksi) and 97 pct.
The thermoelastic micromechanical stresses associated with a single large hexagonal alpha-SiC grain within a fine-grain-size cubic (3C) beta-SiC matrix were calculated. The naturally occurring residual stresses which are created during cooling from the processing temperatures and the effects of superimposed applied external stresses are both considered. A significant effect of the shape or geometry of the alpha-SiC grain is revealed, with the largest residual stresses associated with the naturally occurring tabular or platelet structure. The stresses are compared with the published strength results for these materials, which suggests that the residual stresses assume a significant role in the strength reduction that is observed.
The present 1000 C and 1300 C oxidation tests on 111-oriented single-crystal Si and dense CVD Si3N4 notes the oxidation rates of the latter in wet O2, dry O2, wet inert gas, and steam atmosphere conditions to be several orders of magnitude lower than the rates for the former in identical atmospheric conditions. Although the parabolic rate constant for Si increased linearly as the water vapor pressure increased, the parabolic rate constant for Si3N4 exhibited a nonlinear dependency on water vapor pressure in the presence of O2. NO and NH3 formation at the reaction interface of Si3N4, and the counterpermeation of these reaction products, are noted to dominate reaction kinetics.
A number of commercially available SiC and Si3N4 materials were exposed to 1000 C for 40 h in a high-velocity, pressurized burner rig as a simulation of an aircraft turbine environment. Na impurities (2 ppm) added to the burner flame resulted in molten Na2SO4 deposition, attack of the SiC and Si3N4, and formation of substantial Na2O+x(SiO2) corrosion product. Room-temperature strength of the materials decreased as a result of the formation of corrosion pits in SiC and grain-boundary dissolution and pitting in Si3N4.
The active-to-passive transition in the oxidation of SiC and Si3N4 was determined in a flowing air environment as a function of temperature and total pressure. The experimentally observed transition temperatures ranged from a low of 1347 C to a high of 1543 C for partial pressures of oxygen of 2.5 and 123.2 Pa, respectively. The SiC and Si3N4 samples had approximately the same transition point for a given pressure. In general, the higher the flow rate, the higher the transition temperature for a given pressure. The transitions for SiC measured in this study agree with previous data for the transition of SiC measured in pure oxygen at reduced pressures and in oxygen inert gas mixtures.
An overview of two approaches to the formation of ceramic composite matrices from polymeric precursors is presented. Copolymerization of alkyl- and alkenylsilanes (RSiH3) represents a new precursor system for the production of Beta-SiC on pyrolysis, with copolymer composition controlling polymer structure, char yield, and ceramic stoichiometry and morphology. Polysilsesquioxanes which are synthesized readily and can be handled in air serve as precursors to Si-C-O ceramics. Copolymers of phenyl and methyl silsesquioxanes display rheological properties favorable for composite fabrication; these can be tailored by control of pH, water/methoxy ratio and copolymer composition. Composites obtained from these utilize a carbon coated, eight harness satin weave Nicalon cloth reinforcement. The material exhibits nonlinear stress-strain behavior in tension.
This invention is a method for the controlled growth of single-crystal semiconductor device quality films of SiC polytypes on vicinal (0001) SiC wafers with low tilt angles. Both homoepitaxial and heteroepitaxial SiC films can be produced on the same wafer. In particular, 3C-SiC and 6H-SiC films can be produced within selected areas of the same 6H-SiC wafer.
The stabilities of different phases in the Si-Al-C-O system are calculated from thermodynamic considerations with the objective of identifying the liquid phases formed during sintering of SiC in the presence of Al2O3. It is shown that a liquid phase can form at the sintering temperatures by the reaction of SiC with Al2O3. Depending on the carbon activity, the liquid can be either of the following: Al2O3 + Al4C3, SiC + Al4C3, or molten aluminum. The stability of the aluminosilicate melts that can form by the reaction of Al2O3 with the surface silica layer on SiC powders is also evaluated. Several factors that influence liquid-phase sintering, such as the solubility of SiC in the melts and the generation of gases during sintering, are discussed. The results of the thermodynamic analysis are compared with the observed sintering behavior for SiC.
An overview of two approaches to the formation of ceramic composite matrices from polymeric precursors is presented. Copolymerization of alkyl- and alkenylsilanes (RSiH3) represents a new precursor system for the production of Beta-SiC on pyrolysis, with copolymer composition controlling polymer structure, char yield, and ceramic stoichiometry and morphology. Polysilsesquioxanes which are synthesized readily and can be handled in air serve as precursors to Si-C-O ceramics. Copolymers of phenyl and methyl silsesquioxanes display rheological properties favorable for composite fabrication; these can be tailored by control of pH, water/methoxy ratio and copolymer composition. Composites obtained from these utilize a carbon coated, eight harness satin weave Nicalon cloth reinforcement. The material exhibits nonlinear stress-strain behavior in tension.
The long-term oxidation behavior of pure, monolithic CVD SiC and Si3N4 is studied, and the isothermal oxidation kinetics of these two materials are obtained for the case of 100 hrs at 1200-1500 C in flowing oxygen. Estimates are made of lifetimes at the various temperatures investigated. Parabolic rate constants for SiC are within an order of magnitude of shorter exposure time values reported in the literature. The resulting silica scales are in the form of cristobalite, with cracks visible after exposure. The oxidation protection afforded by silica for these materials is adequate for long service times under isothermal conditions in 1-atm dry oxygen.