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Mieskowski, D. M.

Publications and source records attributed to Mieskowski, D. M..

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.↗

Effect of grain-boundary crystallization on the high-temperature strength of silicon nitride

Si3N4 specimens having the composition 88.7 wt pct Si3N4-4.9 wt pct SiO2-6.4 wt pct Y2O3 were sintered at 2140 C under 25 atm N2 for 1 h and then subjected to a 5 h anneal at 1500 C. Crystallization of an amorphous grain-boundary phase resulted in the formation of Y2Si2O7. The short-time 1370 C strength of this material was compared with that of material of the same composition having no annealing treatment. No change in strength was noted. This is attributed to the refractory nature of the yttrium-rich grain-boundary phase (apparently identical in both glassy and crystalline phases) and the subsequent domination of the failure process by common processing flaws.

Pierce, L. A.↗

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.↗

Reliability of two sintered silicon nitride materials

Two types of sintered silicon nitride were evaluated in terms of reliability: an experimental high pressure nitrogen sintered material and a commercial material. The results show wide variations in strength for both materials. The Weibull moduli were 5.5, 8.9, and 11 for the experimental material at room temperature, 1200, and 1370 C, respectively. The commercial material showed Weibull moduli of 9.0, 8.6, and 8.9 at these respective temperatures. No correlation between strength and flaw size was noted for the experimental material. The applicability of the Weibull and Griffith theories to processing defects on the order of 100 microns or less in size are discussed.

Mieskowski, D. M.↗

Microstructure of reaction-bonded silicon nitride consolidated by isostatic hot-pressing

A microstructural examination and chemical analysis are conducted for reaction-bonded Si3N4 specimens that were isostatically hot pressed at 1850, 1950, and 2050 C. The present observations indicate that the previously reported increase in the 1200 C bend strength of reaction-bonded Si3N4, after pressing at 2050 C exclusively, is due to the relative oxygen levels of the isostatically hot pressed specimens; calculations show that an SiO2 content of less than about 2.2 vol pct is needed to yield the 1200 C strength increase.

Mieskowski, D. M.↗

Oxidation of silicon nitride sintered with rare-earth oxide additions

The effects of rare-earth oxide additions on the oxidation of sintered Si3N4 were examined. Insignificant oxidation occurred at 700 and 1000 C, with no evidence of phase instability. At 1370 C, the oxidation rate was lowest for Y2O3 and increased for additions of La2O3, Sm2O3, and CeO2, in that order. Data obtained from X-ray diffraction, electron microprobe analysis, and scanning electron microscopy indicate that oxidation occurs via diffusion of cationic species from Si3N4 grain boundaries.

Mieskowski, D. M.↗

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.↗

Bubble formation in oxide scales on SiC

The oxidation of alpha-SiC single crystals and sintered alphaand beta-SiC polycrystals has been investigated at elevated temperatures. Bubble formation is commonly observed in oxide scales on polycrystalline SiC, but is rarely found on single-crystal scales; bubbles result from the preferential oxidation of C inclusions, which are abundant in SiC polycrystals. The absence of bubbles on single crystals, in fact, implies that diffusion of the gaseous species formed on oxidation, CO (or possibly SiO), controls the rate of oxidation of SiC.

Mieskowski, D. M.↗