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All sourcesNASA NTRSDOE OSTI
NASA NTRS1977

Pressureless sintered beta-prime-Si3N4 solid solution - Fabrication, microstructure, and strength

Pressureless sintering of beta-prime-Si3N4 solid solution was studied as a function of temperature using Si3N4, A1N, and Al2O3 as basic constituents. Y2O3-SiO2 additions were used to promote liquid-phase sintering. The sintered specimens were characterized with respect to density, microstructure, strength, oxidation, and thermal shock resistance. Density greater than 98 percent of theoretical was achieved by pressureless sintering at 1750 C. The microstructure consisted essentially of fine-grained beta-prime-Si3N4 solid solution as the major phase. Modulus of rupture strengths up to 483 M Pa were achieved at moderate temperature (1000 C), but decreased to 228 M Pa at 1380 C. This substantial strength loss was attributed to a 'glassy' grain boundary phase formed during cooling from the sintering temperature. The best oxidation resistance was exhibited by a composition containing 3 mol % Y2O3-SiO2 additives. Water quench thermal shock resistance was equivalent to that of reaction sintered silicon nitride but lower than hot-pressed silicon nitride.

Dutta, S.↗
NASA NTRS1979

Effect of Si3N4 powder reactivity on the preparation of the Si2N2O-Al2O3 silicon aluminum oxynitride solid solution

Dense high-purity silicon aluminum oxynitride was prepared by reactive hot-pressing of an Si3N4-Al2O3-SiO2 mixture. The formation of a single-phase material was found to be critically dependent on the Si3N4 powder in the starting mixture. It is suggested that evolution of a chlorine- and nitrogen-containing species may enhance the reactivity of Si3N4 in this reaction. Densities of O prime sialons are very similar to that of Si2N2O, the widely quoted value in the ceramics literature of 3.1 g/cu cm for the density of Si2N2O being incorrect.

Sekercioglu, I.↗
NASA NTRS1982

Effects of heating rate on density, microstructure, and strength of Si3N4-6 wt.% Y2O3 and a beta-prime sialon

The effects of the heating rate during sintering/firing on the final density, microstructure, and strength of Si3N4-6 wt% Y2O3 and beta-prime sialon, sintered for four hours at 1750 C, are examined. In Si3N4-6 wt% Y2O3 increasing the heating rate from 7 C/min to 25 C/min to 90 C/min results in a corresponding decrease in the final density from 3.01 g/cu cm to 2.92 g/cu cm to 2.76 g/cu cm. In the beta-prime sialon composition all three heating rates produce an equivalent final density of 3.13 g/cu cm. All heating rates in both compositions produce nonhomogeneous microstructures. The room-temperature strength of Si3N4-6 wt% Y2O3 increases from 372 to 510 MPa with increased density, while the corresponding strengths for the betaprime sialon at equivalent densities are 345 to 445 MPa.

Campbell, S. S.↗
NASA NTRS1983

Analysis of grain boundary phase devitrification of Y2O3- and Al2O3-doped Si3N4

The present study has the objective to show that a Fourier Transform IR (FTIR) spectrometer in a single-beam reflection mode can be used for direct comparison of fractured vs nonfractured Si3N4 surfaces. This can be done because the FTIR method permits a digital summation of nearly 1000 scans of the fracture surface. Commercial-grade Si3N4, Y2O3, and Al2O3 were used in the study. The samples were heat treated in a vacuum induction heating furnace at either 1000 C for 10 h or 1200 C for 10 h each. Use of Fourier transform IR reflection spectroscopic analysis and X-ray diffraction shows that 10 h at 1200 C is sufficient to devitrify the amorphous grain boundary phase of Si3N4 containing 15 percent Y2O3 + 2 percent Al2O3 densification aids.

Hench, L. L.↗
NASA NTRS1984

Microstructure, strength, and oxidation of a 10 wt pct zyttrite-Si3N4 ceramic

Hot pressed Si3N4 doped with 10 wt pct zyttrite as a sintering aid was studied. An equiaxed, fine grained microstructure was predominant, with no apparent porosity. Bend strengths were determined at room temperature and high temperatures (up to 1370 C). Oxidation was measured by weight gain at 1370 C in air. The resulting material exhibited very good room temperature strength (755 MPa). The work showed that room temperature strength can be improved significantly by using controlled Si3N4 powder with 10 wt pct zyttrite. High temperature strength (514 MPa) at 1370 C was nearly double that of hot-pressed Si3N4 (NC-132). The oxidation resistance at 1370 C was also higher than that of NC-132.

Dutta, S.↗
NASA NTRS1986

Strength and microstructure of Si3N4 sintered with ZrO2 additions

Densities greater than 99 percent of theoretical were obtained with stabilized ZrO2 additions to Si3N4. Material sintered at 2140 C under 2.5 MPa nitrogen overpressure with 3.8, 9.9, and 13.4 wt pct ZrO2 had a predominantaly equiaxed grain size ranging from 0.2 to 7.0 microns. At 1370 C, the latter composition exhibited a flexural strength of about 487 MPa, equal to that of a finer-grain-size, hot-pressed Si3N4 + ZrO2 material having excellent high-temperature static fatigue properties. Transmission electron microscopy of the sintered Si3N4 revealed a glassy grain-boundary phase at all three ZrO2 levels and partially crystalline triple points for the 9.9 and 13.4 wt pct ZrO2-containing materials. Slow crack growth was observed for 1370 C flexure tests and correlated with nonlinear load deflection traces for stresses greater than 503 MPa. The crystallization of the grain-boundary glass is insterpreted as beneficial to the attainment of high (1370 C) flexural strength.

Sanders, W. A.↗
NASA NTRS1986

Sintering, microstructural, radiographic, and strength characterization of a high-purity Si3N4-based composition

A commercially available high purity alpha-Si3N4 powder (UBE SN-E10) was characterized, milled with additives, and sintered in a high-pressure nitrogen atmosphere at temperatures ranging from 1750 to 2140 C. The composition selected for this study has been previously examined using a different alpha-Si3N4 powder. Densification behavior, microstructure characteristics, X-radiographic appearance, room- and high-temperatures flexural strength, and fracture-initiating flaw sites were determined. The high-temperature flexural strengths significantly exceeded those observed in the earlier studies using an identical composition (different alpha-Si3N4 powder) and similar processing techniques.

Kiser, J. D.↗
NASA NTRS1991

Oxidation instability of SiC and Si3N4 following thermal excursions

The effect of thermal excursion and thermal cycling on the oxidation stability of chemical vapor-deposited (CVD) SiC and Si3N4 was studied at 1350 C. Thermal cycling alone produced no noticeable change in oxidation kinetics. However, TEM showed that oxide scales grown in cycles consist of alternating layers of SiO2 and Si2N2O. When the oxidation of CVD SiC or Si3N4 at 1350 C was interrupted with a 1.5-h annealing in Ar at 1500 C, the kinetics of reoxidation at 1350 C were found to be drastically increased. The SiC and Si3N4 then oxidized essentially at the same rate, which is over 50 times the preannealing rate, and comparable to the expected oxidation rate of these materials at 1500 C.

Ogbuji, Linus U. J. T.↗
NASA NTRS1993

Mechanism of incipient oxidation of bulk chemical vapor deposited Si3N4

X-ray photoelectron spectroscopy was employed, in conjunction with ion bombardment, to analyze the chemical composition profile across thin (less than 50 nm) oxide films on chemically vapor deposited Si3N4. The thermal oxides were grown in dry oxygen at 1100 C on samples with or without native oxide film (formed in room air). The results show that the thermal oxidation product was silicon oxynitride of graded N:O ratio, and that the presence of a native oxide film promotes the formation of a SiO2 crust over the oxynitride. It is proposed that the fundamental mechanism of Si3N4 oxidation is progressive O-for-N substitution in the silicon oxynitride unit tetrahedron, which is best designated SiN(2-x)O(2+x), where x is also an index of depth. The corresponding equation for nonstoichiometric oxidation of Si3N4 describes a bulk (rather than an interface) reaction process, with significant implications for O2 and N2 fluxes and diffusivities.

Ogbuji, L. U. T.↗
DOE OSTI2020

Materials Data on Si3N4 by Materials Project

Si3N4 crystallizes in the hexagonal P6_3/m space group. The structure is one-dimensional and consists of one Si3N4 ribbon oriented in the (0, 0, 1) direction. there are two inequivalent Si4+ sites. In the first Si4+ site, Si4+ is bonded to four N3- atoms to form a mixture of corner and edge-sharing SiN4 trigonal pyramids. There are a spread of Si–N bond distances ranging from 1.69–1.89 Å. In the second Si4+ site, Si4+ is bonded to four N3- atoms to form a mixture of corner and edge-sharing SiN4 trigonal pyramids. There are a spread of Si–N bond distances ranging from 1.69–1.79 Å. There are three inequivalent N3- sites. In the first N3- site, N3- is bonded in an L-shaped geometry to two equivalent Si4+ atoms. In the second N3- site, N3- is bonded in a rectangular see-saw-like geometry to four Si4+ atoms. In the third N3- site, N3- is bonded in a distorted trigonal planar geometry to three Si4+ atoms.

36 MATERIALS SCIENCE↗
NASA NTRS1979

Consolidation of Si3N4 by hot isostatic pressing

Silicon nitride (Si3N4) is being considered for gas turbine engine applications because present-day metallic alloys are rapidly approaching the limits of their temperature capabilities. The present investigation was undertaken to determine the feasibility of producing a sound, dense Si3N4 body without additives, using conventional gas hot-isostatic-pressing techniques and an uncommon hydraulic hot-isostatic-pressing technique. These two hot-isostatic-pressing (HIP) techniques produce much higher pressure (275-413 MN/sq m) than conventional hot-pressing techniques and have the potential of producing large bodies of desirable shapes. Evaluation was based on density measurement, microscopic examination, both optical and electron, and X-ray diffraction analysis.

Yeh, H. C.↗
NASA NTRS1980

Thermal decomposition of a Si3N4-22 wt% Al2O3 alloy

It is pointed out that materials near the Si3N4 corner of the Si3N4-AlN-Al2O3-SiO2 quaternary, termed sialons are candidate materials for high performance applications. Hot pressed alloys in this system are useful because they possess high flexure strengths and good oxidation and creep resistance. The results of the thermal decomposition studies conducted indicate that dissociation and resulting weight loss lead to inhomogeneous specimens. Material loss comes primarily from near the surface (at least initially) thus causing differences between the composition of the surface material and the bulk. In these specimens, the O-prime phase was found to be the least stable to dissociation and the beta-prime phase the most stable. This result is in accord with the conclusions of Mitomo et al. (1979) that Si2N2O has a larger equilibrium SiO partial pressure than either the X phase or the beta-prime phase.

Ditchek, B. M.↗
NASA NTRS1984

The impact resistance of SiC and other mechanical properties of SiC and Si3N4

Studies focused on the impact and mechanical behavior of SiC and Si3N4 at high temperatures are summarized. Instrumented Charpy impact testing is analyzed by a compliance method and related to strength; slow crack growth is related to processing, and creep is discussed. The transient nature of flaw populations during oxidation under load is emphasized for both SiC and Si3N4.

Bradt, R. C.↗
NASA NTRS1983

Hardness of dense beta-Si3N4

The effects of small changes in the concentration of an oxygen content densification aid on the room temperature microhardness of hot isostatically pressed and sintered beta-Si3N4 ceramics are studied. The compositions studied were Si3N4 containing 7 wt. pct BeSiN2, a fixed nonoxide densification aid, and 1.9-3.7 wt. pct oxygen as a second, variable densification aid. A proportional relationship between high density and high oxygen content, regardless of heat treatment type, is noted.

Greskovich, C.↗
NASA NTRS1983

Characteristics of Si3N4-SiO2-Ce2O3 compositions sintered in high-pressure nitrogen

Full-density Si3N4-SiO2-Ce2O3 compositions were prepared by sintering with 2.5 MPa nitrogen pressure at temperatures of 1900 and 2090 C. Room-temperature flexural strengths near 700 MPa for sintered material compared favorably with the strength of hot-pressed material. At 1370 C, where flexural strengths as high as 363 MPa were obtained, it was observed that the coarsest structure was the strongest and the finest structure was the weakest. One of the compositions tested, Si3N4-8.7 wt pct SiO2-8.3 wt pct-Ce2O3, was found to have excellent 200-h oxidation resistance at 700, 1000, and 1370 C, without incidence of 700 to 1000 C phase instability and cracking.

Sanders, W. A.↗
NASA NTRS1984

Demonstration of a silicon nitride attrition mill for production of fine pure Si and Si3N4 powders

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.

Herbell, T. P.↗
NASA NTRS1985

Strength and microstructure of sintered Si3N4 with rare-earth-oxide additions

Room temperature, 700-, 1000-, 1200-, and 1370-C examinations of the effect of 1.7-2.6 mol pct rare earth oxide additions to sintered Si3N4 are conducted. While the room temperature-1000 C bend strengths were higher for this material with Y2O3 additions than with CeO2, La2O3, or Sm2O3, the reverse was true at 1200-1370 C. This phenomenon is explained on the basis of microstructural differences, since quantitative microscopy of SEM replicas showed the Si3N4-Y2O3 composition to contain both a higher percentage of elongated grains and a coarser microstructure than the other three alternatives. The elongated grains appear to increase this composition's low temperature strength irrespective of microstructural coarseness; this coarseness, however, decreases strength relative to the other compositions at higher temperatures.

Sanders, W. A.↗