Cavitation Contributes Substantially to Tensile Creep in Silicon Nitride

During tensile creep of a hot isostatically pressed (HIPed) silicon nitride, the volume fraction of cavities increases linearly with strain; these cavities produce nearly all of the measured strain. In contrast, compressive creep in the same stress and temperature range produces very little cavitation. A stress exponent that increases with stress (ε∞σ ⁿ , 2 < n < 7) characterizes the tensile creep response, while the compressive creep response exhibits a stress dependence of unity. Furthermore, under the same stress and temperature, the material creeps nearly 100 times faster in tension than in compression. Transmission electron microscopy (TEM) indicates that the cavities formed during tensile creep occur in pockets of residual crystalline silicate phase located at silicon nitride multigrain junctions. Small-angle X-ray scattering (SAXS) from crept material quantifies the size distribution of cavities observed in TEM and demonstrates that cavity addition, rather than cavity growth, dominates the cavitation process. These observations are in accord with a model for creep based on the deformation of granular materials in which the microstructure must dilate for individual grains to slide past one another. During tensile creep the silicon nitride grains remain rigid; cavitation in the multigrain junctions allows the silicate to flow from cavities to surrounding silicate pockets, allowing the dilatation of the microstructure and deformation of the material. Silicon nitride grain boundary sliding accommodates this expansion and leads to extension of the specimen. In compression, where cavitation is suppressed, deformation occurs by solution—reprecipitation of silicon nitride.     

Tensile Creep and Rupture of Silicon Nitride

We have characterized the tensile creep, rupture lifetime, and cavitation behavior of a commercial, gas-pressure-sintered silicon nitride in the temperature range 1150° to 1400°C and stress range 70 to 400 MPa. Individual creep curves generally show primary, secondary, and tertiary creep. The majority of the primary creep is not recoverable. The best representation of the data is one where the creep rate depends exponentially on stress, rather than on the traditional power law. This representation also removes the need to break the data into high and low stress regimes. Cavitation of the interstitial silicate phase accompanies creep under all conditions, and accounts for nearly all of the measured strain. These observations are consistent with a model where creep proceeds by the redistribution of silicate phase from cavitating interstitial pockets, accommodated by grain-boundary sliding of silicon nitride.     

Tensile Creep and Creep Rupture Behavior of Monolithic and SiC-Whisker-Reinforced Silicon Nitride Ceramics

The tensile creep and creep rupture behavior of silicon nitride was investigated at 1200° to 1350°C using hotpressed materials with and without SiC whiskers. Stable steady-state creep was observed under low applied stresses at 1200°C. Accelerated creep regimes, which were absent below 1300°C, were identified above that temperature. The appearance of accelerated creep at the higher temperatures is attributable to formation of microcracks throughout a specimen. The whisker-reinforced material exhibited better creep resistance than the monolith at 1200°C; however, the superiority disappeared above 1300°C. Considerably high values, 3 to 5, were obtained for the creep exponent in the overall temperature range. The exponent tended to decrease with decreasing applied stress at 1200°C. The primary creep mechanism was considered cavitationenhanced creep. Specimen lifetimes followed the Monkman–Grant relationship except for fractures with large accelerated creep regimes. The creep rupture behavior is discussed in association with cavity formation and crack coalescence.     

Creep mechanisms in quasi-plastic silicon nitride by instrumented indentation

Quasi-plastic creep behavior of the commercial, fine-grained silicon nitride grade, ST 1, was investigated using variety of techniques with the focus on the analysis of instrumented indentation. Creep deformation in this material was characterized by high creep rates at temperatures above 1300 °C and failure strains around 20%. It was accompanied by strong oxidation, cracking of the oxide layers, excessive cavitation at multigrain junctions and slight texture formation. Instrumented indentation revealed degradation of indentation moduli in the oxide layers and enhancement of oxidation and elastic moduli degradation during creep. Because of the similarities between the mass transport processes in cavitation, diffusion processes involved in oxidation and similar activation energies, both creep and oxidation occur simultaneously, however, oxidation is enhanced by external stress. Texture formation implied from disappearance of -silicon nitride and anisotropy of indentation modulus contributes insignificantly (<5%) to total tensile strain. Creep processes in the studied material can be explained within the expanded cavitation creep model of Luecke and Wiederhorn assuming that cavitation is facilitated by low viscosity residual glass and small matrix grain size. Tertiary-like creep is attributed to the gradual increase of the applied stress resulting from the reduction of the effective cross section due to the formation of cracked oxide layers. Size and pre-oxidation effects were predicted and confirmed using creep samples with different gauge size.     

Creep and Creep Rupture of an Advanced Silicon Nitride Ceramic

Creep and creep rupture behavior of an advanced silicon nitride ceramic were systematically characterized in the temperature range 1150° to 1300°C using uniaxial tensile creep tests. Absence of tertiary creep and the order-of-magnitude breaks in both creep rate and rupture lifetime at certain threshold combinations of stress and temperature were two characteristic features of the creep behavior observed. Thermal annealing was found to have enhanced both subsequent creep resistance and creep rupture life. The stress exponent (n) and the activation energy (Q) defined in the Norton relation were found to be 12.6 and 1645 kJ/mol for the material investigated. Both values appear to fall in the general range of those reported for other but similar types of Si₃N₄ ceramic materials. The stress exponent, m , equivalent to the slope of the Larson–Miller equation was found to be in the range 13 to 14.4, and that defined as p in the Monkman–Grant relation to be 0.91, based on the available experimental data. The values of m , n , and p obtained above approximately support the interrelationship of the three exponents given by p = m/n.     

Creep and Stress Rupture Behavior of an Advanced Silicon Nitride: Part I, Experimental Observations

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.     

Tensile Creep Behavior of a Vitreous-Bonded Aluminum Oxide under Static and Cyclic Loading

Creep deformation and rupture behavior of a vitreousbonded aluminum oxide was investigated under uniaxial static and cyclic tensile loadings at 1000°, 1100°, and 1175°C. The material was more creep resistant, i.e., having lower creep strain rates, under cyclic loading compared to that under static loading. For the same maximum applied stress, the ratio of steady-state creep rate under static loading to that under cyclic loading at 1100°C was approximately 100. However, the value of this ratio decreased to about 10 when the testing temperature was raised to 1175°C or lowered to 1000°C. Under static loading the material had more propensity to develop creep damage in the form of micro- and macrocracks, leading to early failure, whereas under cyclic loading the creep damage was more uniformly distributed in the form of cavities confined to the multigrain junctions. Viscous bridging by the grain boundary second phase may be the primary contributor to the lower creep deformation rate and improved lifetime under cyclic loading.     

Results of an International Round-Robin for Tensile Creep Rupture of Silicon Nitride

Fourteen laboratories participated in an interlaboratory study to establish the within- and between-laboratory repeatability of tensile creep rupture of silicon nitride. In air at 1375°C at 200 MPa, the times to failure ranged over a factor of 50, and the minimum creep rates ranged over a factor of 20. Despite these large ranges, taken individually, no one laboratory stands out from any other; all produced equally acceptable data. Consumers of silicon nitride tensile creep data must accept this magnitude of variability in reported creep data. The wide variety of specimen shapes and sizes, gripping systems, extensometry techniques, and temperature measurement strategies makes it impossible to assign definitively the root cause of the variability. However, there was a significant specimen size effect. As a group, the small-diameter specimens lasted roughly five times longer and crept three times more slowly than the large-diameter buttonhead specimens. A possible interpretation of the origin of this difference is that the oxidizing conditions affected more of the volume of the small specimens during the test.     

Creep and Stress–Strain Behavior after Creep for SiC Fiber Reinforced, Melt-Infiltrated SiC Matrix Composites

Silicon carbide fiber (Hi-Nicalon Type S, Nippon Carbon) reinforced silicon carbide matrix composites containing melt-infiltrated silicon were subjected to creep at 1315°C at three different stress conditions. For the specimens that did not rupture after 100 h of tensile creep, fast-fracture experiments were performed immediately following the creep test at the creep temperature (1315°C) or after cooling to room temperature. All specimens demonstrated excellent creep resistance and compared well to the creep behavior published in the literature on similar composite systems. Tensile results on the after-creep specimens showed that the matrix cracking stress actually increased, which is attributed to stress redistribution between composite constituents during tensile creep.     

Tensile Creep Behavior of a Gas-Pressure-Sintered Silicon Nitride Containing Silicon Carbide

The tensile creep behavior of a gas-pressure-sintered silicon nitride containing silicon carbide was characterized at temperatures between 1375° and 1450°C with applied stresses between 50 and 250 MPa. Individual specimens were tested at fixed temperatures and applied loads. Each specimen was pin-loaded within the hot zone of a split-tube furnace through silicon carbide rods connected outside the furnace to a pneumatic cylinder. The gauge length was measured by laser extensometry, using gauge markers attached to the specimen. Secondary creep rates ranged from 0.54 to 270 Gs⁻¹, and the creep tests lasted from 6.7 to 1005 h. Exponential functions of stress and temperature were fitted to represent the secondary creep rate and the creep lifetime. This material was found to be more creep resistant than two other silicon nitride ceramics that had been characterized earlier by the same method of measurement as viable candidates for high-temperature service.     

Evaluation of the Strength and Creep–Fatigue Behavior of Hot Isostatically Pressed Silicon Nitride

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.     

Apparent Enhanced Fatigue Resistance under Cyclic Tensile Loading for a HIPed Silicon Nitride

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 (<175 MPa) originated from environmentally assisted (oxidation) and generalized creep damage, while failures at similar times but much greater (up to 2 x) cyclic stresses originated from preexisting defects (slow crack growth failures). At 1370°C, stress rupture results did not show as pronounced differences between static, dynamic, and cyclic loading conditions, with most failures originating from environmentally assisted (oxidation) and generalized creep damage.     

Ultrasonic Velocity Technique for Nondestructive Quantification of Elastic Moduli Degradation during Creep in Silicon Nitride

The ultrasonic velocity technique was used for nondestructive quantification of creep damage during interrupted tensile creep tests at 1400°C in an advanced silicon nitride to investigate the possibilities of this technique for creep damage monitoring in ceramic components. The longitudinal and shear wave velocities, Poisson's ratio, and Young's, shear, and bulk moduli linearly decreased with strain. Precise density change measurements indicated a linear relationship with a coefficient of proportionality of 0.69 between the volume fraction of cavities and tensile strain. Cavitation was identified as the main creep mechanism in the studied silicon nitride and the reason for ultrasonic velocity and elastic moduli degradation. The measurement of just the longitudinal wave velocity changes was found to be sufficient for quantification of cavitation during creep. The capability of the ultrasonic velocity technique for simple, sensitive, and reliable nondestructive monitoring of creep damage during intermittent creep was demonstrated in silicon nitride.     

Comparison of Tensile and Compressive Creep Behavior in Silicon Nitride

The creep behavior of a commercial grade of Si₃N₄ was studied at 1350° and 1400°C. Stresses ranged from 10 to 200 MPa in tension and from 30 to 300 MPa in compression. In tension, the creep rate increased linearly with stress at low stresses and exponentially at high stresses. By contrast, the creep rate in compression increased linearly with stress over the entire stress range. Although compressive and tensile data exhibited an Arrhenius dependence on temperature, the activation energies for creep in tension, 715.3 ± 22.9 kJ/mol, and compression, 489.2 ± 62.0 kJ/mol, were not the same. These differences in creep behavior suggests that mechanisms of creep in tension and compression are different. Creep in tension is controlled by the formation of cavities. The cavity volume fraction increased linearly with increased tensile creep strain with a slope of unity. A cavitation model of creep, developed for materials that contain a triple-junction network of second phase, rationalizes the observed creep behavior at high and low stresses. In compression, cavitation plays a less important role in the creep process. The volume fraction of cavities in compression was ∼18% of that in tension at 1.8% axial strain and approached zero at strains <1%. The linear dependence of creep rate on applied stress is consistent with a model for compressive creep involving solution–precipitation of Si₃N₄. Although the tensile and compressive creep rates overlapped at the lowest stresses, cavity volume fraction measurements showed that solution–precipitation creep of Si₃N₄ did not contribute substantially to the tensile creep rate. Instead, cavitation creep dominated at high and low stresses.     

Flexural Stress Rupture and Creep of Selected Commercial Silicon Nitrides

Four commercial Si₃N₄ compositions were compared with regard to flexural stress rupture and creep in ambient air as functions of temperature from 1100° to 1400°C and stress from 200 to 350 MPa. One Si₃N₄, SN252, was found to be more resistant to time-dependent deformation in both stepped-temperature stress rupture tests and creep tests than a very similar Si₃N₄ composition and two other dissimilar Si₃N₄ compositions. Materials were compared on the bases of percent final strains, creep rates, and posttest microscope examinations. The latter revealed tensile face transverse cracking, and slow crack growth. The superior behavior of the SN252 Si₃N₄ was related to its microstructure.     

Effect of Creep Damage on the Tensile Creep Behavior of a Siliconized Silicon Carbide

The tensile creep behavior of a siliconized silicon carbide was investigated in air, under applied stresses of 103 to 172 MPa for the temperature range of 1100° to 1200°C. At 1100°C, the steady-state stress exponent for creep was approximately 4 under applied stresses less than the threshold for creep damage (132 MPa). At applied stresses greater than the threshold stress for creep damage, the stress exponent increased to approximately 10. The activation energy for steady-state creep at 103 MPa was approximately 175 kJ/mol for the temperature range of 1100° to 1200°C. Under applied stresses of 137 and 172 MPa, the activation energy for creep increased to 210 and 350 kJ/mol, respectively, for the same temperature range. Creep deformation in the siliconized silicon carbide below the threshold stress for creep damage was determined to be controlled by dislocation processes in the silicon phase. At applied stresses above the threshold stress for creep damage, creep damage enhanced the rate of deformation, resulting in an increased stress exponent and activation energy for creep. The contribution of creep damage to the deformation process was shown to increase the stress exponent from 4 to 10.     

Role of Oxidation in the Time-Dependent Failure Behavior of Hot Isostatically Pressed Silicon Nitride at 1370°C

Dynamic fatigue studies were conducted on a hot isostatically pressed silicon nitride in ambient air and inert (argon or nitrogen) environments using four-point flexure at 1370°C. Specimens tested in ambient air exhibited a stressing rate dependence with decreased flexure strength with decreased stressing rates. All fracture surfaces of specimens tested in ambient air possessed a sweeping stress-oxidation damage zone that originated at the tensile side of each bend bar. In addition to this stress-oxidation damage, creep damage (e.g., cavitation) was concurrently observed in the specimens tested at the slower stressing rates, which appeared to further weaken the material. However, tests conducted in argon or nitrogen revealed flexure strength to be independent of the stressing rate. Creep damage was present at the slower stressing rates, but no stress-oxidation damage was evident similar to that observed on the specimens tested in ambient air. By decoupling the effects of oxidation and creep, it was evident that the former contributed to the formation of a detrimental stress-oxidation damage zone which significantly reduced the strength of this material at 1370°C.     

Observed and Theoretical Creep Rates for an Alumina Ceramic and a Silicon Nitride Ceramic in Flexure

Observed creep curvature rates are compared to theoretical rates for both an alumina ceramic at 1000°C and a silicon nitride ceramic at 1200°C in four-point flexure. The observed rates have been calculated from published rise-displacement rates, and the theoretical rates have been calculated from published power-law parameters for compressive and tensile creep, which differ appreciably for these ceramics. Although both compressive and tensile creep measurements are easier to analyze than flexural creep measurements, the latter are usually less expensive and easier to conduct. The present work shows the usefulness of flexural creep tests to verify the accuracy of compressive and tensile creep tests.     

Creep and Stress Rupture Behavior of an Advanced Silicon Nitride: Part II, Creep Rate Behavior

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.     

Damage-Enhanced Creep in a Siliconized Silicon Carbide: Phenomenology

The creep behavior of a commercial grade of reaction-bonded silicon carbide was characterized at a temperature of 1300°C. Creep occurred more easily in tension than in compression. At a given applied stress, the steady-state creep rate in tension was found to be at least 20 times that obtained in compression. In both tension and compression, the stress exponent for steadystate creep was found to increase with increasing applied stresses. At low applied stresses, the stress exponent was ∼4, suggesting some kind of dislocation mechanism operating in the two-phase composite. At high stresses, the stress exponent was ∼11 in tension. The increase in the stress exponent was attributed to damage accumulation in the form of cavities. An effective threshold stress for cavitation of less than 100 MPa was suggested. In compression, the cause of the increase of stress exponent with stress cannot be attributed to cavitation.