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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.

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.

Statistical techniques are used to derive closed-form, approximate solutions for estimating a standard deviation on the fracture stress determined from mirror size measurements. The estimated coefficient of variation of fracture stress is noted to be twice as sensitive to the variation of the mirror constant, Aj, as to the variation in the measured boundary radius, r j . This allows the hackle radius to be reasonably estimated and bounded from the mirror and branch radii when it cannot be clearly delineated.

Cylindrical buttuohead specimens of an advanced silicon nitride were tested in uniaxial tension at temperatures between 1422 and 1673 K. In the range 1477 to 1673 K, creep deformation was reliably measured using high-temperature contact probe extensometry. Extensive scanning and transmission electron microscopy has revealed the formation of lenticular cavities at two-grain junctions at all temperatures (1422–1673 K) and extensive triple-junction cavitation occurring at the higher temperatures (1644–1673 K). Cavitation is believed to be part of the net creep process. The stress rupture data show stratification of the Monkman–Grant lines with respect to temperature. Failure strain increased with increase in rupture time or temperature, or decrease in stress. Fractography showed that final failure occurred by subcritical crack growth in all specimens.

In Part I of this paper, experimental observations on creep testing of 74 tensile specimens of an advanced silicon nitride were presented. In this part, equations are developed for predicting creep rates in the primary and secondary regimes in the temperature range 1477–1673 K. The resulting model predicts creep strain rates to within a factor of two. The underlying phenomenological basis, which employs an activation energy approach, is discussed. The mechanisms that are likely to be responsible for the transiency of the primary creep regime and for the unique stress and temperature dependencies of the creep rates are explored.

The applicability of the Monkman-Grant relationship to predict the stress rupture life of NT154 silicon nitride is examined. The data show that the Monkman-Grant lines relating rupture life to minimum creep rate are stratified with respect to temperature. A modification to the current expression for the Monkman-Grant relation is proposed to accommodate this temperature dependence. A phenomenological approach based on crack growth as the failure mechanisms is presented to explain this temperature dependence. The results can be interpreted as suggesting that the stress dependence of the failure process is greater than that for creep.

Measurements of the tensile creep and creep rupture behavior were used to evaluate the long-term mechanical reliability of a commercially available and a developmental hot isostatically pressed (HIPed) silicon nitride. Measurements were conducted at 1,260 and 1,370 C utilizing button-head tensile specimens. The stress and temperature sensitivities of the secondary creep rates were used to estimate the stress exponent and activation energy associated with the dominant creep mechanism. The stress and temperature dependencies of creep rupture life were determined by continuing individual creep tests to specimen failure. Creep deformation in both materials was associated with cavitation at multigrain junctions. Two-grain cavitation was also observed in the commercial material. Failure in both materials resulted from the evolution of an extensive damage zone. The failure times were uniquely related to the creep rates, suggesting that the zone growth was constrained by the bulk creep response. The fact that the creep and creep rupture behaviors of the developmental silicon nitride were significantly improved compared to those of the commercial material was attributed to the absence of cavitation along two-grain junctions in the developmental material.

Cyclic tensile loading tests of a commercial HIPed silicon nitride at elevated temperatures have indicated apparent “enhanced” fatigue resistance compared to static tensile loading tests under similar test conditions. At 1150°C, stress rupture results plotted as maximum stress versus time to failure did not show significant differences in failure behavior between static, dynamic, or cyclic loading conditions, with all failures originating from preexisting defects (slow crack growth failures). At 1260°C, the stress rupture results showed pronounced differences between static, dynamic, and cyclic loading conditions. Failures at low static stresses (

The strength of a commericially available hot isostatically pressed silicon nitride was measured as a function of temperature. To evaluate long-term mechanical reliability of this material, the tensile creep and fatigue behavior was measured at 1150°, 1260°, and 1370°C. The stress and temperature sensitivities of the secondary (or minimum) creep strain rate were used to estimate the stress exponent and activation energy associated with the dominant creep mechanism. The fatigue characteristics were evaluated by allowing individual creep tests to continue until specimen failure. The applicability of the four-point load geometry to the study of strength and creep behavior was also determined by conducting a limited number of flexural creep tests. The tensile fatigue data revealed two distinct failure mechanisms. At 1150°C, failure was controlled by a slow crack growth mechanism. At 1260° and 1370°C, the accumulation of creep damage in the form of grain boundary cavities and cracks dominated the fatigue behavior. In this temperature regime, the fatigue life was controlled by the secondary (or minimum) creep strain rate in accordance with the Monkman–Grant relation.

The fracture resistance of a fully dense, transparent, polycrystalline magnesium aluminate spinel was measured from room temperature to 1400°C using the chevron-notched beam and the straight-notched beam macroflaw techniques, as well as the indentation-induced, controlled-microflaw test method, all in three-point bending. Flexural strengths were also measured for the same range of temperatures to compare with the fracture toughness measurements. From the load vs load-line displacement (P-u) curves of the chevronnotched test specimens, the crack growth resistance curves (R-curves) and the total work-of-fracture were determined. It was observed that polycrystalline MgAl2O4 exhibits rising R-curve behavior which increases with increasing test temperature. The R-curve increases are attributed to the geometric constraints due to grain bridging and grain wedging phenomena as well as secondary grain boundary microcracking processes, all of which occurred in the wake region behind the advancing crack. The work-of-fracture and the R-curves increased rapidly above 800°C coincident with the onset of increased secondary grain boundary microcracking.

The fracture toughness of a dense, sintered commercial α-silicon carbide was determined for temperatures from 20° to 1400°C using both straight- and chevron-notched test specimens and also controlled-surface-microflaw specimens, all in three-point bending. The flexural strengths were also measured for the same range of temperatures and the trend is compared with that of the toughness. Measurements from this study are discussed and also compared with other results in the literature. Analysis reveals the importance of contrasting sharp crack and blunt crack techniques and also the need for addressing the microhardness indentation method separately. It is concluded that the fracture toughness of this silicon carbide is about 3 MPa · m½ and that the crack growth resistance is characterized by a flat R-curve behavior, both of which are independent of temperature from 20° to 1400°C.

The fracture initiation and arrest stress intensity factors were determined for a SiC-whisker-reinforced AI2O3 matrix composite. A chevron-notched, three-point-bend specimen was used to genera e the load/displacement curve, which exhibited repeated crack initiation, followed by crack arrest behavior. Corresponding stress intensity factors were determined for both situations using the compliance technique. Calculated crack arrest positions were in agreement with fractographic observations. Both the crack arrest and the crack initiation stress intensity factors exhibited a rising R -curve with increasing crack length, suggesting the presence of wake toughening effects on the crack growth resistance.