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Oxidation resistance, and examples of oxidation of SiC, Si3N4 and sialon are reviewed. A description is given of the oxidation mechanism, including the oxidation product, oxidation reaction and the bubble size. The oxidation reactions are represented graphically. An assessment is made of the oxidation process, and an oxidation example of silicon ceramics is given.
The development of a beam-leaded low power, high performance metal-oxide-semiconductor (MOS), 256-bit random access memory (RAM) was reported. Previous success with the aluminum-gate current-sense version and a silicon-gate voltage-sense version led to the present effort to make a beam-leaded silicon-gate RAM. Some problems unique to the silicon-on-sapphire beam-lead process development are presented. Beam-leaded SOS TA5388 devices using a Si3N4 passivation layer were shown to have good electrical parameters.
Silicon epitaxy analysis of silane produced in the Process Development Unit operating in a completely integrated mode consuming only hydrogen and metallurgical silicon resulted in film resistivities of up to 120 ohms cm N type. Preliminary kinetic studies of dichlorosilane disproportionation in the liquid phase have shown that 11.59% SiH4 is formed at equilibrium after 12 minutes contact time at 56 C. The fluid-bed reactor was operated continuously for 48 hours with a mixture of one percent silane in helium as the fluidizing gas. A high silane pyrolysis efficiency was obtained without the generation of excessive fines. Gas flow conditions near the base of the reactor were unfavorable for maintaining a bubbling bed with good heat transfer characteristics. Consequently, a porous agglomerate formed in the lower portion of the reactor. Dense coherent plating was obtained on the silicon seed particles which had remained fluidizied throughout the experiment.
An uncooled infrared tunneling sensor in which the only moving part is a diaphragm which is deflected into contact with a micromachined silicon tip electrode prepared by a novel lithographic process. Similarly prepared deflection electrodes employ electrostatic force to control the deflection of a silicon nitride, flat diaphragm membrane. The diaphragm exhibits a high resonant frequency which reduces the sensor's sensitivity to vibration. A high bandwidth feedback circuit controls the tunneling current by adjusting the deflection voltage to maintain a constant deflection of the membrane which would otherwise change deflection depending upon incident infrared radiation. The resulting infrared sensor will meet or exceed the performance of all other broadband, uncooled, infrared sensors and can be miniaturized to pixel dimensions smaller than 100 .mu.m. The technology is readily implemented as a small-format linear array suitable for commercial and spacecraft applications.
An uncooled infrared tunneling sensor in which the only moving part is a diaphragm which is deflected into contact with a micromachined silicon tip electrode prepared by a novel lithographic process. Similarly prepared deflection electrodes employ electrostatic force to control the deflection of a silicon nitride, flat diaphragm membrane. The diaphragm exhibits a high resonant frequency which reduces the sensor's sensitivity to vibration. A high bandwidth feedback circuit controls the tunneling current by adjusting the deflection voltage to maintain a constant deflection of the membrane. The resulting infrared sensor can be miniaturized to pixel dimensions smaller than 100 .mu.m. An alternative embodiment is implemented using a corrugated membrane to permit large deflection without complicated clamping and high deflection voltages. The alternative embodiment also employs a pinhole aperture in a membrane to accommodate environmental temperature variation and a sealed chamber to eliminate environmental contamination of the tunneling electrodes and undesireable accoustic coupling to the sensor.
This report summarizes work performed in support of the development and demonstration of a structural ceramic technology for automotive gas turbine engines. The AGT101 regenerated gas turbine engine developed under the previous DOE/NASA Advanced Gas Turbine (AGT) program is being utilized for verification testing of the durability of next-generation ceramic components and their suitability for service at reference powertrain design conditions. Topics covered in this report include ceramic processing definition and refinement, design improvements to the test bed engine and test rigs, and design methodologies related to ceramic impact and fracture mechanisms. Appendices include reports by ATTAP subcontractors addressing the development of silicon nitride and silicon carbide families of materials and processes.
Reinforced carbon-carbon material specimens were machined from 19 and 33 ply flat panels which were fabricated and processed in accordance with the specifications and procedures accepted for the fabrication and processing of the leading edge structural subsystem (LESS) elements for the space shuttle orbiter. The specimens were then baseline coated and tetraethyl orthosilicate impregnated, as applicable, in accordance with the procedures and requirements of the appropriate LESS production specifications. Three heater bars were ATJ graphite silicon carbide coated with the Vought 'pack cementation' coating process, and three were stackpole grade 2020 graphite silicon carbide coated with the chemical vapor deposition process utilized by Vought in coating the LESS shell development program entry heater elements. Nondestructive test results are reported.
This report is the fourth in a series of Annual Technical Summary Reports for the Advanced Turbine Technology Applications Project (ATTAP). This report covers plans and progress on ceramics development for commercial automotive applications over the period 1 Jan. - 31 Dec. 1991. Project effort conducted under this contract is part of the DOE Gas Turbine Highway Vehicle System program. This program is directed to provide the U.S. automotive industry the high-risk, long-range technology necessary to produce gas turbine engines for automobiles with reduced fuel consumption, reduced environmental impact, and a decreased reliance on scarce materials and resources. The program is oriented toward developing the high-risk technology of ceramic structural component design and fabrication, such that industry can carry this technology forward to production in the 1990s. The ATTAP test bed engine, carried over from the previous AGT101 project, is being used for verification testing of the durability of next-generation ceramic components, and their suitability for service at Reference Powertrain Design conditions. This document reports the technical effort conducted by GAPD and the ATTAP subcontractors during the fourth year of the project. Topics covered include ceramic processing definition and refinement, design improvements to the ATTAP test bed engine and test rigs and the methodology development of ceramic impact and fracture mechanisms. Appendices include reports by ATTAP subcontractors in the development of silicon nitride and silicon carbide families of materials and processes.
This invention relates to a process comprising the steps of: a) providing a fiber preform comprising a non-oxide ceramic fiber with at least one coating, the coating comprising a coating element selected from the group consisting of carbon, nitrogen, aluminum and titanium, and the fiber having a degradation temperature of between 1400.degree. C. and 1450.degree. C., b) impregnating the preform with a slurry comprising silicon carbide particles and between 0.1 wt % and 3 wt % added carbon c) providing a cover mix comprising: i) an alloy comprising a metallic infiltrant and the coating element, and ii) a resin, d) placing the cover mix on at least a portion of the surface of the porous silicon carbide body, e) heating the cover mix to a temperature between 1410.degree. C. and 1450.degree. C. to melt the alloy, and f) infiltrating the fiber preform with the melted alloy for a time period of between 15 minutes and 240 minutes, to produce a ceramic fiber reinforced ceramic composite.
New process uses paint sprayer and vacuum furnace to produce silicon carbide outer layer. In cross section of silicon and silicon carbide reaction zone, top layer of silicon adheres to silicon carbide layer. Crystals prominent on melted top surface of slurry coating. Process especially useful in coating repair.
A process for transferring an entire wafer-level micromachined silicon structure for mating with and bonding to another such structure has been devised. This process is intended especially for use in wafer-level integration of microelectromechanical systems (MEMS) that have been fabricated on dissimilar substrates. Unlike in some older membrane-transfer processes, there is no use of wax or epoxy during transfer. In this process, the substrate of a wafer-level structure to be transferred serves as a carrier, and is etched away once the transfer has been completed. Another important feature of this process is that two electrodes constitutes an electrostatic actuator array. An SOI wafer and a silicon wafer (see Figure 1) are used as the carrier and electrode wafers, respectively. After oxidation, both wafers are patterned and etched to define a corrugation profile and electrode array, respectively. The polysilicon layer is deposited on the SOI wafer. The carrier wafer is bonded to the electrode wafer by using evaporated indium bumps. The piston pressure of 4 kPa is applied at 156 C in a vacuum chamber to provide hermetic sealing. The substrate of the SOI wafer is etched in a 25 weight percent TMAH bath at 80 C. The exposed buried oxide is then removed by using 49 percent HF droplets after an oxygen plasma ashing. The SOI top silicon layer is etched away by using an SF6 plasma to define the corrugation profile, followed by the HF droplet etching of the remaining oxide. The SF6 plasma with a shadow mask selectively etches the polysilicon membrane, if the transferred membrane structure needs to be patterned. Electrostatic actuators with various electrode gaps have been fabricated by this transfer technique. The gap between the transferred membrane and electrode substrate is very uniform ( 0.1 m across a wafer diameter of 100 mm, provided by optimizing the bonding control). Figure 2 depicts the finished product.
The Solid-state Prealkylation of Electrode ARchitectures (SPEAR) is different than traditional electrochemical prealkylation processes. Through SPEAR, alkylation is driven by solid-state diffusion without the simultaneous SEI formation concomitant with polarization. Here, we investigate the prelithiation of 80 wt. % Si-based anodes to varying amounts (up to Li 1.38 Si) to understand the trade-off between improved Li capacity and expansion-induced stress. Through dilatometry, we found that solid-state lithiation led to filling of the electrode pores through silicon expansion. This swelling changed the SEI formation process and accessibility of the silicon compared to an electrochemically lithiated electrode. Indeed, optimal prelithiation to Li 0.82 Si increases the initial C/3 cycling capacity post-SEI formation up to 43%, consistent with deeper Si activation through the electrode bulk. Prelithiation and cycling cells prelithiated beyond Li 0.82 Si results in a state of charge (SOC) close to 100% which facilitates parasitic degradation mechanisms and volume expansion of the Si electrode. The results demonstrate a pathway to modify silicon activation/SEI formation to enable high-energy electrodes.
The reliability of microfocus x-radiography and scanning laser acoustic microscopy for detecting microvoids in silicon nitride and silicon carbide was statistically evaluated. Materials- and process-related parameters that influenced the statistical findings in research samples are discussed. The use of conventional x-radiography in controlling and optimizing the processing and sintering of an Si3N4-Si02-Y203 composition designated NASA 6Y is described. Radiographic evaluation and guidance helped develop uniform high-density Si3N4 modulus-of-rupture bars with improved four-point flexural strength (857, 544, and 462 MPa at room temperature, 1200 C, and 1370 C, respectively) and reduced strength scatter.
The reliability of microfocus X-radiography and scanning laser acoustic microscopy for detecting microvoids in silicon nitride and silicon carbide was statistically evaluated. Materials- and process-related parameters that influenced the statistical findings in research samples are discussed. The use of conventional X-radiography in controlling and optimizing the processing and sintering of an Si3N4-SiO2-Y2O3 composition designated NASA 6Y is described. Radiographic evaluation and guidance helped develop uniform high-density Si3N4 modulus-of-rupture bars with improved four-point flexural strength (857, 544, and 462 MPa at room temperature, 1200 C, and 1370 C, respectively) and reduced strength scatter.
A program to develop a power processing system for ion thrusters is presented. Basic operation of the silicon controlled rectifier series inverter circuitry is examined. The approach for synthesizing such circuits into a system which limits the electrical stress levels on the power source, semiconductor switching elements, and the ion thruster load is described. Experimental results are presented for a 2.5-kW breadboard system designed to operate a 20-cm ion thruster.
Inside diametar wafering equipment, blades and processes were used to develop methods to produce large areas of silicon sheet. Modifications to a 16 inch STC automated saw included: programmable feed system, crystal rotating system, and STC dynatrack blade monitoring and control system. By controlling the plating operation and by grinding of the cutting edge, 16 inch ID blades with a cutting edge thickness of .22 mm can be produced. 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 ID slicing techniques. Using programmed feeds and programmed rotation, maximum cutting rates were from 0.3 to 1.0 inches per minute.
Thick film silicon ribbons were produced by means of the edge-defined, film-fed growth (EFG) technique. EFG is a process by which single crystals may be grown having a shape controlled by the outside dimensions of a die, the growth taking place from an extremely thin film of liquid fed by capillary action from a crucible below. The principal problem to be overcome in the application of this process to the growth of thick film silicon ribbon relates to the material, such as the shaping die. For the method to operate, this die material must be wet by the liquid silicon. To preserve semiconductor quality, the liquid silicon must not react significantly with the die material. The most promising die material for this application appears to be SiC and SiC-SiO2 admixture. In this case good wetting occurs between the molten silicon and the SiC. C is a relatively unharmful contaminant of Si and additions of quartz to SiC are found to decrease the extent of reaction.
The present invention relates to organic silicon-boron polymers which upon pyrolysis produce high-temperature ceramic materials. More particularly, it relates to the polyorganoborosilanes containing -Si-B- bonds which generate high-temperature ceramic materials (e.g., SiC, SiB4, B4C) upon thermal degradation. The process for preparing these organic silicon-boron polymer precursors are also part of the invention.