Effect of starting powder characteristics on density, microstructure and low temperature oxidation behavior of a Si3N4 - 8 w/o Y2O3 ceramic
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Schuon, S.↗
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Oxidation stability of advanced reaction-bonded Si3N4 materials
Four slip-cast, injection-molded and isostatically-pressed specimens of reaction-bonded silicon nitride (RBSN) were subjected to static oxidation tests at 900 C for 10 hours. Specimens containing 8-10% interconnected open porosity of size greater than one micron exhibited a 20-30% decrease in average room temperature four-point flexure strength, while those with 10% open porosity of magnitudes much smaller than one micron as well as those with 2-4% interconnected open porosity of about one micron did not decrease in strength after 900 C exposure. It was determined that preoxidation treatment at 1350 C prevents the 20-30% strength degradation due to internal oxidation, and evidence is presented which suggests that surface pit formation in some RBSN may result from contamination by the furnace environment rather than any intrinsic material properties.
Lindberg, L. J.↗
The effect of silicon particle size on the nitriding behaviour of reaction bonded Si3N4 compacts
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Mangels, J. A.↗
Conformal step coverage of electron beam-assisted CVD of SiO2 and Si3N4 films
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Thompson, L. R.↗
Use of plasma-deposited Si3N4 as an oxidation mask in the fabrication of GaAs shallow-homojunction solar cells
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Turner, G. W.↗
Mechanical properties of SiC fiber-reinforced reaction-bonded Si3N4 composites
The room temperature mechanical and physical properties of silicon carbide fiber reinforced reaction-bonded silicon nitride composites (SiC/RBSN) have been evaluated. The composites contained 23 and 40 volume fraction of aligned 140 micro m diameter chemically vapor deposited SiC fibers. Preliminary results for composite tensile and bend strengths and fracture strain indicate that the composites displayed excellent properties when compared with unreinforced RBSN of comparable porosity. Fiber volume fraction showed little influence on matrix first cracking strain but did influence the stressed required for matrix first cracking and for ultimate composite fracture strength. It is suggested that by reducing matrix porosity and by increasing the volume fraction of the large diameter SiC fiber, it should be possible to further improve the composite stress at which the matrix first cracks.
Bhatt, R. T.↗
Iron impurities in Si3N4 processing
The atomic environment of iron impurities is investigated during the processing cycle of reaction-bonding silicon nitride (RBSN). Several analysis techniques are utilized, including X-ray photoelectron spectroscopy (XPS), extended X-ray absorption fine structure (EXAFS), and electron spin resonance (ESR), to examine iron impurities in the starting silicon powder, in sintered silicon compacts, and in RBSN materials. Results indicate that iron impurities in as-received metallurgical grade silicon powder are incorporated in the silicon bulk as a highly distorted FeSi2 compound. No surface iron or iron-based particulate is observed in the starting material. Upon sintering, the iron environment becomes an ordered FeSi2 structure. In the RBNS material, the FeSi2 structure is again distorted, as observed by both EXAFS and ESR.
Bouldin, C. E.↗
Mechanical properties of SiC fiber-reinforced reaction-bonded Si3N4 composites
The room temperature mechanical and physical properties of silicon carbide fiber reinforced reaction-bonded silicon nitride composites (SiC/RBSN) have been evaluated. The composites contained 23 and 40 volume fraction of aligned 140 micro m diameter chemically vapor deposited SiC fibers. Preliminary results for composite tensile and bend strengths and fracture strain indicate that the composites displayed excellent properties when compared with unreinforced RBSN of comparable porosity. Fiber volume fraction showed little influence on matrix first cracking strain but did influence the stressed required for matrix first cracking and for ultimate composite fracture strength. It is suggested that by reducing matrix porosity and by increasing the volume fraction of the large diameter SiC fiber, it should be possible to further improve the composite stress at which the matrix first cracks.
Bhatt, Ramakrishna T.↗
Optimization of Processing of Si3N4
Process changes iterated under guidance of x-radiography. In recent work at NASA Lewis Research Center, density gradients in sintered silicon nitride, characterized by x-radiography, identified and appeared strongly dependent upon powder-processing and sintering conditions. NASA technical memorandum describes systematic investigation, based upon preliminary work, of density-gradient/flexural-strength relationships as affected by processing.
Sanders, William A.↗
Molten salt corrosion of SiC and Si3N4
The most severe type of corrosion encountered in heat engines is corrosion by molten sodium sulfate, formed by the reaction of ingested sodium chloride and sulfur impurities in the fuel. This problem was studied extensively for superalloys, but only recently examined for ceramics. This problem is addressed with laboratory studies to understand the fundamental reaction mechanisms and with burner studies to provide a more realistic simulation of the conditions encountered in a heat engine. In addition the effect of corrosion on the strengths of these materials was assessed. Each of these aspects will be reviewed and some ideas toward possible solutions will be discussed.
Jacobson, N. S.↗
The high temperature creep deformation of Si3N4-6Y2O3-2Al2O3
The creep properties of silicon nitride containing 6 wt percent yttria and 2 wt percent alumina have been determined in the temperature range 1573 to 1673 K. The stress exponent, n, in the equation epsilon dot varies as sigma sup n, was determined to be 2.00 + or - 0.15 and the true activation energy was found to be 692 + or - 25 kJ/mol. Transmission electron microscopy studies showed that deformation occurred in the grain boundary glassy phase accompanied by microcrack formation and cavitation. The steady state creep results are consistent with a diffusion controlled creep mechanism involving nitrogen diffusion through the grain boundary glassy phase.
Todd, J. A.↗
Molten salt corrosion of SiC and Si3N4
Industrial systems such as heat engines and heat exchangers involve harsh environments. The structural materials are subjected to high temperatures as well as corrosive gases and condensed phases. Past experience with metal alloys has shown that these condensed phases can be particularly corrosive and are often the limiting factor in the operation of these systems. In a heat engine the most common condensed corrodent is Na2SO4 whereas in a heat exchanger an oxide slag may be present. The primary emphasis is on Na2SO4 induced corrosion, however, similarities and differences to oxide slag are also discussed. The extensive research on corrosion of metal alloys has led to understanding and controlling corrosion for these materials. Currently silicon based ceramics are prime candidates for the applications discussed. Therefore it is important to understand the effects of condensed phase deposits on this emerging class of high temperature materials. Both the thermodynamic and strength of the ceramic is also examined. Finally some control strategies for corrosion of silicon based ceramics are explored.
Jacobson, Nathan S.↗
The behavior of SiC and Si3N4 ceramics in mixed oxidation/chlorination environments
The behavior of silicon-based ceramics in mixed oxidation/chlorination environments was studied. High pressure mass spectrometry was used to quantitatively identify the reaction products. The quantitative identification of the corrosion products was coupled with thermogravimetric analysis and thermodynamic equilibrium calculations run under similar conditions in order to deduce the mechanism of corrosion. Variations in the behavior of the different silicon-based materials are discussed. Direct evidence of the existence of silicon oxychloride compounds is presented.
Marra, John E.↗
Electron beam induced damage in PECVD Si3N4 and SiO2 films on InP
Phosphorus rich plasma enhanced chemical vapor deposition (PECVD) of silicon nitride and silicon dioxide films on n-type indium phosphide (InP) substrates were exposed to electron beam irradiation in the 5 to 40 keV range for the purpose of characterizing the damage induced in the dielectic. The electron beam exposure was on the range of 10(exp -7) to 10(exp -3) C/sq cm. The damage to the devices was characterized by capacitance-voltage (C-V) measurements of the metal insulator semiconductor (MIS) capacitors. These results were compared to results obtained for radiation damage of thermal silicon dioxide on silicon (Si) MOS capacitors with similar exposures. The radiation induced damage in the PECVD silicon nitride films on InP was successfully annealed out in an hydrogen/nitrogen (H2/N2) ambient at 400 C for 15 min. The PECVD silicon dioxide films on InP had the least radiation damage, while the thermal silicon dioxide films on Si had the most radiation damage.
Pantic, Dragan M.↗
The high temperature creep deformation of Si3N4-6Y2O3-2Al2O3
The creep properties of silicon nitride containing 6 wt percent yttria and 2 wt percent alumina have been determined in the temperature range 1573 to 1673 K. The stress exponent, n, in the equation epsilon dot varies as sigma sup n, was determined to be 2.00 + or - 0.15 and the true activation energy was found to be 692 + or - 25 kJ/mol. Transmission electron microscopy studies showed that deformation occurred in the grain boundary glassy phase accompanied by microcrack formation and cavitation. The steady state creep results are consistent with a diffusion controlled creep mechanism involving nitrogen diffusion through the grain boundary glassy phase.
Todd, J. A.↗
Nitriding kinetics of Si-SiC powder mixtures as simulations of reaction bonded Si3N4-SiC composites
The nitriding kinetics of Si and Si plus SiC powder mixtures were studied to simulate the fabrication of RBSN-SiC ceramic matrix composites. Very clean, assynthesized, and solvent-exposed powders were studied; C-rich and Si-rich SiC 0.04-0.05 micron diameter powders were mixed in varying concentrations with SiH4-derived 0.2-0.3 micron diameter Si powder. Complete nitridation is achieved with C-rich SiC powders in 140 min at 1250 C, and in the centers of Si-rich SiC powders in 15 min. The effects on the incubation periods, fast reaction periods, and slow reaction periods that characterize these nitriding processes were studied to explain unusual reverse reaction gradients and other effects of contamination.
Lightfoot, A.↗
Si3N4 emissivity and the unidentified infrared bands
Infrared spectroscopy of warm (about 150 to 750 K), dusty astronomical sources has revealed a structured emission spectrum which can be diagnostic of the composition, temperature, and in some cases, even size and shape of the grains giving rise to the observed emission. The identifications of silicate emission in oxygen rich objects and SiC in carbon rich object are two examples of this type of analysis. Cometary spectra at moderate resolution have similarly revealed silicate emission, tying together interstellar and interplanetary dust. However, Goebel has pointed out that some astronomical sources appear to contain a different type of dust which results in a qualitatively different spectral shape in the 8 to 13 micron region. The spectra shown make it appear unlikely that silicon nitride can be identified as the source of the 8 to 13 micron emission in either NGC 6572 or Nova Aql 1982. The similarity between the general wavelength and shape of the 10 micron emission from some silicates and that from the two forms of silicon nitride reported could allow a mix of cosmic grains which include some silicon nitride if only the 8 to 13 micron data are considered.
Russell, Ray W.↗
Gibbs free energy of reactions involving SiC, Si3N4, H2, and H2O as a function of temperature and pressure
Silicon carbide and silicon nitride are considered for application as structural materials and coating in advanced propulsion systems including nuclear thermal. Three-dimensional Gibbs free energy were constructed for reactions involving these materials in H2 and H2/H2O. Free energy plots are functions of temperature and pressure. Calculations used the definition of Gibbs free energy where the spontaneity of reactions is calculated as a function of temperature and pressure. Silicon carbide decomposes to Si and CH4 in pure H2 and forms a SiO2 scale in a wet atmosphere. Silicon nitride remains stable under all conditions. There was no apparent difference in reaction thermodynamics between ideal and Van der Waals treatment of gaseous species.
Isham, M. A.↗