Library

Notes: Two commercially available additive-containing silicon nitride materials were exposed in four environments which ranged in severity from dry oxygen at 1 atm pressure, and low gas velocity, to an actual turbine engine. Oxidation and volatilization kinetics were monitored at temperatures ranging from 1066° to 1400°C. The main purpose of this paper is to examine the surface oxide morphology resulting from the exposures. It was found that the material surface was enriched in rare-earth silicate phases in combustion environments when compared with the oxides formed on materials exposed in dry oxygen. However, the in situ formation of rare-earth disilicate phases offered little additional protection from the volatilization of silica observed in combustion environments. It was concluded that externally applied environmental barrier coatings are needed to protect additive-containing silicon nitride materials from volatilization reactions in combustion environments.

Notes: The work reported was conducted to provide a basis for a number of structural ceramic mechanical property standardization activities in the United States, Germany, Japan, and Sweden. A comparison of key property values of a commercial silicon nitride determined in a number of laboratories was a major objective. The work reported was conducted by 10 U.S. laboratories on GN-10 silicon nitride, and represented the U.S. work within an International Energy Agency program including the United States, Germany, Japan, and Sweden. Fracture location analyses showed that fracture location within the inner span often was not a linear function of location within the span. Some of this behavior was explained by random sampling effects based upon simulation predictions, but some was apparently dependent upon friction within the fixtures in spite of efforts to minimize it. Flexural strengths were measured at 25° and 1250°C in air and were analyzed using the two-parameter Weibull model in terms of m and σΘ using both linear regression (LR) and maximum likelihood (ML) methods. Under the measurement conditions for the 10 room-temperature strength sets, the value of the ML estimator for m varied by as much as 36%, while the value for the σΘ parameter estimator varied only 3.3%. The LR estimator for m varied by about 54%. For the high-temperature specimens, the ML estimator for m varied by 48% while the LR estimator varied by 38%. Ranked fracture location analysis showed that the high-temperature fracture locations were more random than those in the room-temperature specimens, and was probably due to friction in the high-temperature fixtures. There was little pin rolling ability in many of the high-temperature fixtures used. Monte Carlo and one-way analysis-of-variance (ANOVA) methods provided insight into the consistency of the strength values. Monte Carlo predictions showed that for room-temperature strength, the maximum likelihood estimator m for all 10 laboratories fit within the 10% and 90% confidence bounds for 30 specimen sets. The dispersion of the high-temperature data was such that the m estimator satisfied the model only at the 1% and 99% confidence levels for the 15 specimen sets. ANOVA results showed that for the room-temperature flexural strength, data from all 10 laboratories were not distinguishable for this evaluator at the 95% confidence level and that scatter within individual data sets was a larger effect than was the variation between the data sets. For the high-temperature data, the results from one laboratory were clearly outside the allowable range at this confidence level.

Notes: Crystalline mullite was deposited by chemical vapor deposition (CVD) onto SiC/SiC composites overlaid with CVD SiC. Specimens were exposed to isothermal oxidation tests in high-pressure air + H2O at 1200°C. Unprotected CVD SiC formed silica scales with a dense amorphous inner layer and a thick, porous, outer layer of cristobalite. Thin coatings (∼2 μm) of dense CVD mullite effectively suppressed the rapid oxidation of CVD SiC. No microstructural evidence of mullite volatility was observed under these temperature, pressure, and low-flow-rate conditions. Results of this preliminary study indicate that dense, crystalline, high-purity CVD mullite is stable and protective in low-velocity, high-pressure, moisture-containing environments.

Notes: The work reported was conducted to provide a basis for structural ceramic mechanical property standardization activities under way in the United States, Germany, Japan, and Sweden. All measurements reported here were conducted by 10 U.S. groups on GN-10 silicon nitride within an International Energy Agency program including the United States, Germany, Japan, and Sweden. This cooperative work included tensile strength studies of two geometries of button-head tensile specimens. The authors conducted some of the measurements and performed data analyses and interpretation. The tensile fracture behavior of GN-10 silicon nitride was studied at room temperature. A total of 150 strain-gaged button-head tensile specimens were measured. One hundred of a straight collet design and 50 of a tapered collet design were fractured. All specimens were highly strain gaged and the outputs for each were measured during loading to fracture. Bending moments were calculated. Each participating laboratory group fractured 15 tensile specimens, 10 of the straight collet design and 5 of the tapered collet design under rigorously controlled testing conditions. Of 100 straight collet specimens 75 broke in the gage section. Of 50 tapered collet specimens 34 broke within the gage section. Analysis of the Weibull m and σΘ estimators at upper and lower confidence bounds of 95% and 5% did not indicate a clear choice between the two designs. For specimens which fractured in the gage section, the unbiased maximum likelihood Weibull estimators for m and σΘ were 12.5 and 730 and 10.4 and 716, for the straight and tapered collet configurations, respectively. These are not statistically different at the 95% and 5% confidence levels. Strengths were also analyzed in terms of a three-parameter Weibull model. The straight collet specimen data fitted the three parameter model well with a threshold stress estimator γ of 506 MPa, while the tapered collet specimens provided a poorer fit to the model and had a threshold stress estimator of 432 MPa, a difference of about 15%. Regression analysis indicated that the straight collet grip provided less bias of strength as a function of bending moment. The straight collet specimens showed essentially little dependence of tensile strength upon bending moment in the range of 0% to 6%, while the tapered collet specimens showed a decrease in strength as the bending moment increased from 0% to 4%. However, the regression parameter was low and no significant statistical conclusion could be made regarding the superiority of either of the grip designs.

Notes: Using a newly developed object-oriented finite-element analysis method, both an actual microstructure and model microstructures of a plasma-sprayed thermal barrier coating system were numerically simulated to analyze the full-field residual stresses of this coating system. Residual stresses in the actual microstructure were influenced by both the irregular top-coat/bond-coat interface and cracks in the top coat. By treating the microcracked top coat as a more-compliant solid microstructure, the effects of the irregular interface on residual stresses were examined. These results then could be compared to results that have been obtained by analyzing a model microstructure with a sinusoidal interface, which has been considered by some earlier investigators.

Notes: Dynamic fatigue and stress rupture tests in four-point bending were conducted on a commercially available SN88 silicon nitride ceramic at temperatures in the range 700°–1000°C in air. The objective of the present study was to elucidate the failure of SN88 silicon nitride ceramic nozzles arising from a critical crack initiated at the intermediate temperature airfoil region during an engine field test. Results of dynamic fatigue tests indicated that SN88 silicon nitride tested at a stressing rate of 30 MPa/s exhibited little change in characteristic strength at the various test temperatures. However, SN88 silicon nitride exhibited a significant degradation in mechanical strength when tested at 0.003 MPa/s at temperatures indicative of a great susceptibility to slow crack growth, especially at 850°C. SEM and XRD analyses indicated that the mechanical instability of SN88 silicon nitride at intermediate temperatures resulted from the transformation of secondary phase(s) from oxidation. These phase transformations were accompanied by a large volume change, which led to the generation of large local residual tensile stresses. As a result, extensive damage zones were formed, which led to a substantial degradation of mechanical strength and reliability. Microstructural examination of failed SN88 airfoils indicated that a similar damage zone was formed in the regions exposed to intermediate temperatures during engine testing. Consequently, the ultimate failure of these vanes was attributed to the loss in mechanical strength from the damage zone formation.

Notes: A study of the exposure of SiC at 1200°C and high water-vapor pressures (1.5 atm) has shown SiC recession rates that exceed what is predicted based on parabolic oxidation at water-vapor pressures of less than or equal to ∼1 atm. After exposure to these conditions, distinct silica-scale structures are observed; thick, porous, nonprotective cristobalite scales form above a thin, dense silica layer. The porous cristobalite thickens with exposure time, while the thickness of the underlying dense layer remains constant. These observations suggest a moving-boundary phenomenon that is controlled by the rapid conversion of dense vitreous silica to a porous, nonprotective crystalline SiO2.

Notes: The interfacial characteristics of SiC/C/SiC composites with different fiber-coating bond strengths have been investigated using single-fiber push-out tests. Previous studies have shown that weak or strong bonds can be obtained by using as-received or treated fibers, respectively, and that the stress-strain behavior is improved with the treated fibers. This effect results from multiple branching of the cracks within the interphase. The model used to extract interfacial characteristics from nanoindentation and microindentation tests does not consider the presence of an interphase. However, the results highlight the significant effect of the interphase on the interfacial parameters, as well as the effect of roughness along the sliding surfaces. For the composite with treated fibers, the uncommon upward curvature of the push-out curves is related to different modes of crack propagation in the interphase. Different techniques are required to analyze the interfacial properties, such as nanoindentation and microindentation with push-out and push-back tests.

Notes: A thermal-shock strength-testing technique has been developed that uses a high-resolution, high-temperature infrared camera to capture a specimen's surface temperature distribution at fracture. Aluminum nitride (AlN) substrates are thermally shocked to fracture to demonstrate the technique. The surface temperature distribution for each test and AlN's thermal expansion are used as input in a finite-element model to determine the thermal-shock strength for each specimen. An uncensored thermal-shock strength Weibull distribution is then determined. The test and analysis algorithm show promise as a means to characterize thermal shock strength of ceramic materials.

Notes: The interfacial properties of SiC/SiC composites with interphases that consist of (C-SiC) sequences deposited on the fibers have been determined by single-fiber push-out tests. The matrix has been reinforced with either as-received or treated Nicalon fibers. The measured interfacial properties are correlated with the fiber-coatingbond strength and the number of interlayers. For the composites reinforced with as-received (weakly bonded) fibers, interfacial characteristics are extracted from the nonlinear portion of the stress-displacement curve by fitting Hsueh's push-out model. The interfacial characteristics are controlled by the carbon layer adjacent to the fiber. The resistance to interface crack growth and fiber sliding increases as the number of (C-SiC) sequences increases. For the composites reinforced with treated (strongly bonded) fibers, the push-out curves exhibit an uncommon upward curvature, which reflects different modes of interphase cracking and a contribution of fiber roughness.