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Promising route toward production of highly pure, finely divided, easily sinterable silicon nitride (Si3N4) involves thermal decomposition of silicon diimide {Si(NH)2} prepared by ammonolysis of Si(SCN)4 in CH3CN and purified by complete extraction of byproduct NH4SCN by use of ammonia at temperature and pressure above critical point.
A baseline slurry-pressing method for a silicon nitride material is developed. The Si3N4 composition contained 5.8 wt percent SiO2 and 6.4 wt percent Y2O3. Slurry-pressing variables included volume percent solids, application of ultrasonic energy, and pH. Twenty vol percent slurry-pressed material was approximately 11 percent stronger than both 30 vol percent slurry-pressed and dry-pressed materials. The Student's t-test showed the difference to be significant at the 99 percent confidence level. Twenty volume percent (300 h) slurry-pressed test bars exhibited strengths as high as 980 MPa. Large, columnar beta-Si3N4 grains caused failure in the highest strength specimens. The improved strength correlated with better structural uniformity as determined by radiography, optical microscopy, and image analysis.
A baseline slurry-pressing method for a silicon nitride material is developed. The Si3N4 composition contained 5.8 wt percent SiO2 and 6.4 wt percent Y2O3. Slurry-pressing variables included volume percent solids, application of ultrasonic energy, and pH. Twenty vol percent slurry-pressed material was approximately 11 percent stronger than both 30 vol percent slurry-pressed and dry-pressed materials. The Student's t-test showed the difference to be significant at the 99 percent confidence level. Twenty volume percent (300 h) slurry-pressed test bars exhibited strengths as high as 980 MPa. Large, columnar beta-Si3N4 grains caused failure in the highest strength specimens. The improved strength correlated with better structural uniformity as determined by radiography, optical microscopy, and image analysis.
The effect of the microstructure of reaction bonded silicon nitride on strength is examined. The morphologies of the various microconstituents (alpha-matte, beta-spikes, residual silicon and porosity) each play a role in determining the strength of the material. While density and hence percent porosity greatly affect strength, it is shown that the pore size and pore size distribution affect strength with equal importance. By minimizing the pore size and distribution and maximizing the alpha-beta ratio, a reaction bonded material (2.4 kg/cu m) has been produced with a room temperature modulus of rupture (three-point bending) of 297 MPa from a low green density starting material (1.5 kg/cu m).
To avoid metallic impurities normally introduced by milling ceramic powders in conventional steel hardware, an attrition mill (high-energy stirred ball mill) was constructed with the wearing parts (mill body, stirring arms, and media) made from silicon nitride. Commercial silicon and Si3N4 powders were milled to fine uniform particles with only minimal contamination - primarily from wear of the sintered Si3N4 media.
Transformation of structural ceramics from the laboratory to production requires development of near net shape fabrication techniques which minimize finish grinding. One potential technique for producing large quantities of complex-shaped parts at a low cost, and microstructure of sintered silicon nitride fabricated by injection molding is discussed and compared to data generated from isostatically dry-pressed material. Binder selection methodology, compounding of ceramic and binder components, injection molding techniques, and problems in binder removal are discussed. Strength, oxidation resistance, and microstructure of sintered silicon nitride fabricated by injection molding is discussed and compared to data generated from isostatically dry-pressed material.
Electron radiation stability of silicon nitride insulated gate FET with passivation layers and heat treatment, noting contamination effects
Radiation effects on silicon nitride insulated gate field effect transistors
Feasibility study looks at effectiveness of silicon nitride passivation coating against moisture and mobile ions. Coating was tested on CMOS microcircuits. Tests included temperature cycling, high-temperature electrical stress, and temperature and humidity exposure. Report concludes plastic-encapsulated circuits with protective coating exhibit high survival rates; it includes tables summarizing test results and figures that show effects of flexing.
The strength and crack growth characteristics of a sintered silicon nitride were studied at 1000 C. Fractographic analysis of material failing in dynamic fatigue revealed the presence of slow crack growth (SCG) at stressing rates below 6 ksi/min. This material can sustain a 40-ksi flexural stress at 1000 C for 400 h or more but is susceptible to both SCG and creep deformation at higher stress levels. The crack velocity exponent (N) determined both from dynamic and static fatigue experiments lies in a range from 13 to 22. The subcritical crack growth and creep behavior at 1000 C is primarily controlled by the deformation of an intergranular glassy phase.
The AiResearch Casting Company baseline silicon nitride (92 percent GTE SN-502 Si sub 3 N sub 4 plus 6 percent Y sub 2 O sub 3 plus 2 percent Al sub 2 O sub 3) was characterized with methods that included chemical analysis, oxygen content determination, electrophoresis, particle size distribution analysis, surface area determination, and analysis of the degree of agglomeration and maximum particle size of elutriated powder. Test bars were injection molded and processed through sintering at 0.68 MPa (100 psi) of nitrogen. The as-sintered test bars were evaluated by X-ray phase analysis, room and elevated temperature modulus of rupture strength, Weibull modulus, stress rupture, strength after oxidation, fracture origins, microstructure, and density from quantities of samples sufficiently large to generate statistically valid results. A series of small test matrices were conducted to study the effects and interactions of processing parameters which included raw materials, binder systems, binder removal cycles, injection molding temperatures, particle size distribution, sintering additives, and sintering cycle parameters.
The strength and toughness of two composite and two monolithic silicon nitrides were measured from 25 to 1400 C. The monolithic and composite materials were made from similar starting powders. Both of the composite materials contained 30 vol percent silicon carbide whiskers. All measurements were made by four point flexure in surrounding air and humidity. The composite and monolithic materials exhibited similar fast fracture properties as a function of temperature.
The bearings used in the space shuttle main engine (SSME) high pressure oxidizer turbopump (HPOTP) do not meet the expected life goals that were set for them. In an effort to improve their performance, many solutions are being studied. New bearing materials are being developed, better manufacturing techniques are being investigated, and improved cage materials for better lubrication are being tested. The focus is on the replacement of steel balls with ones made of silicon nitride in 57-mm HPOTP bearings. The bearings were then installed in a test rig and run at near turbopump operating conditions. The results from this test series are encouraging, with silicon nitride showing good wear resistance and thermal stability.
Multilayer plasma-enhanced chemical vapor deposition (PECVD) silicon nitride antireflection coatings were deposited on space quality silicon solar cells. Preliminary experiments indicated that multilayer coatings decreased the total reflectance of polished silicon from 35 percent to less than 3 percent over the spectral range 0.4-1.0 micron. The solar cell energy conversion efficiency was increased from an average of 8.84 percent to an average of 12.63 percent.
The subcritical growth of cracks from pre-existing flaws in ceramics can severely affect the structural reliability of a material. The ability to directly observe subcritical crack growth and rigorously analyze its influence on fracture behavior is important for an accurate assessment of material performance. A Mode I fracture specimen and loading method has been developed which permits the observation of stable, subcritical crack extension in monolithic and toughened ceramics. The test specimen and procedure has demonstrated its ability to generate and stably propagate sharp, through-thickness cracks in brittle high modulus materials. Crack growth for an aluminum oxide ceramic was observed to be continuously stable throughout testing. Conversely, the fracture behavior of a silicon nitride ceramic exhibited crack growth as a series of subcritical extensions which are interrupted by dynamic propagation. Dynamic initiation and arrest fracture resistance measurements for the silicon nitride averaged 67 and 48 J/sq m, respectively. The dynamic initiation event was observed to be sudden and explosive. Increments of subcritical crack growth contributed to a 40 percent increase in fracture resistance before dynamic initiation. Subcritical crack growth visibly marked the fracture surface with an increase in surface roughness. Increments of subcritical crack growth loosen ceramic material near the fracture surface and the fracture debris is easily removed by a replication technique. Fracture debris is viewed as evidence that both crack bridging and subsurface microcracking may be some of the mechanisms contributing to the increase in fracture resistance. A Statistical Fracture Mechanics model specifically developed to address subcritical crack growth and fracture reliability is used together with a damaged zone of material at the crack tip to model experimental results. A Monte Carlo simulation of the actual experiments was used to establish a set of modeling input parameters. It was demonstrated that a single critical parameter does not characterize the conditions required for dynamic initiation. Experimental measurements for critical crack lengths, and the energy release rates exhibit significant scatter. The resulting output of the model produces good agreement with both the average values and scatter of experimental measurements.
NASA Glenn Research Center is developing advanced technology for Stirling convertors with a target of significantly improving the specific power and efficiency of the convertor and overall generator for Mars rovers and deep space missions. One specific approach to the target has been recognized as the use of appropriate high-temperature materials. As a series of ceramic material approaches in Advanced Stirling Convertor Development Program in fiscal year 2005, two commercial, structural silicon nitrides AS800 (Honeywell, Torrence, California) and SN282 (Kyocera, Vancouver, Washington) were selected and their mechanical and life limiting properties were characterized at 1050 C in air. AS800 exhibited both strength and Weibull modulus greater than SN282. A life limiting phenomenon was apparent in AS800 with a low slow crack growth parameter n = 15; whereas, a much increased resistance to slow crack growth was found in SN282 with n greater than 100. Difference in elastic modulus and thermal conductivity was negligible up to 1200 C between the two silicon nitrides. The same was true for the coefficient of thermal expansion up to 1400 C.
A description is given of a sintering method for silicon nitride. A detailed explanation of the invention is presented. Four procedures for the sintering process are described.
The development of silicon carbide-silicon nitride fibers (SiC-Si3N4) by the pyrolysis of polycarbosilazane precursors is reviewed. Precursor resin, which was prepared by heating tris(N-methylamino)methylsilane or tris(N-methylamino)phenylsilane to about 520 C, was drawn into fibers from the melt and then made unmeltable by humidity conditioning at 100 C and 95 percent relative humidity. The humidity treated precursor fibers were pyrolyzed to ceramic fibers with good mechanical properties and electrical resistivity. For example, SiC-Si3N4 fibers derived from tris(N-methylamino)methylsilane had a tensile rupture modulus of 29 million psi and electrical resistivity of 6.9 x ten to the 8th power omega-cm, which is ten to the twelfth power times greater than that obtained for graphite fibers.