Cavity Development During Creep Deformation in Alumina with a Bimodal Grain Size Distribution

An alumina sample, codoped with equimolar proportions of magnesia and zirconia, exhibited a bimodal grain size distribution after hot-pressing. Flexural creep experiments were performed on this material at temperatures of 1673 and 1773 K in air. Inspection of the deformed specimens revealed extensive creep cavitation, with cavities developing preferentially in the coarse-grained regions. The nucleation, growth, and interlinkage of the cavities led to the formation of cracks. Crack growth occurred in the coarse-grained regions by the linkage of cavities with the crack tip. However, several cracks were observed to terminate after extending up to a fine-grained region of a specimen. A model has been developed to rationalize the observation that preferential cavitation occurs in the coarse-grained regions of a specimen undergoing creep deformation.     

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.     

Measurement of Crack Tip Toughness in Alumina as a Function of Grain Size

Crack profile measurements near the crack tip in the SEM were used to measure crack tip toughness of alumina as a function of grain size (average grain size 0.9–16 μm). For comparative tests, two crack configurations were included in the present study: straight cracks (CT specimen) loaded with an in situ device; and radial indentation cracks. The measured crack tip toughness values were independent of crack geometry, and no grain size dependence could be discerned. A mean crack tip toughness of 2.3 MPam^1/2 was evaluated. The crack tip toughness determined from crack profile measurements is significantly lower than the toughness evaluated with conventional indentation techniques (e.g., indentation strength bending).     

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.     

Comparison of High-Temperature Crack Growth in SiC-Whisker-Reinforced Mullite and Si3N4

Crack growth behavior under creep conditions was studied in SiC-whisker-reinforced mullite and silicon nitride. Tests of four-point bend specimens with indentation cracks were periodically interrupted to observe the creep behavior. At each interruption the bulk creep strain of the specimen, the growth of the indentation cracks, and the nucleation and growth of creep-induced cracks were measured. A strong linear correlation was observed in both materials between the crack growth rate and the creep strain rate. For a given strain rate, cracks in the silicon nitride composite propagated at velocities about an order of magnitude greater than those in the mullite composite. On the other hand, for similar nominal stresses, creep rates in the silicon nitride composites were about an order of magnitude less than with the mullite composite.     

Damage and Fracture Mechanisms During High-Temperature Creep in Hot-Pressed Alumina

The mechanisms responsible for creep damage accumulation and fracture have been examined in two commercial hot-pressed aluminas. Differences between the two materials can be ascribed to minor compositional variations. Three damage regimes have been identified, depending on stress. However, in all three regimes, failure is controlled by crack propagation. At high stress, a single crack, nucleated at a processing flaw, controls failure. These cracks grow in a linear elastic stress field. At intermediate stresses, crack tip stresses relax, and many microcracks are nucleated. They grow and link under strain control. The details of this process differ under tension and bending, thus invalidating the flexure test as a means of establishing creep life, even in simple, single-phase materials. At the lowest stress, extensive cavitation, with relatively little microcrack development, is observed. However, failure continues to be dominated by the growth of cracks. The material is damage tolerant and can be thought of as superplastic. We find that processing flaws (primarily large grains) control the creep life at all stresses. These should therefore be carefully controlled in materials aimed at high-temperature structural applications.     

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.     

Nucieation and Growth of Cracks in Vitreous-Bonded Aluminum Oxide at Elevated Temperatures

The nucleation and growth of cracks was studied at elevated temperatures on a grade of vitreous-bonded aluminum oxide that contained ∼8 vol% glass at the grain boundaries. Cracks were observed to nucleate within the vitreous phase, close to the tensile surface of the flexural test specimens used in these experiments. Crack nucleation occurred at a strain of ∼0.08% to 0.12% which corresponded to a crack nucleation time of ∼35% of the time to failure by creep rupture. Once nucleated, cracks propagated along grain boundaries, as long as the stress for crack propagation was maintained. The crack velocity for cracks that were nucleated by the creep process was found to be linearly proportional to the apparent stress intensity factor, whereas for cracks that were nucleated by indentation, the crack velocity was proportional to the fourth power of the apparent stress intensity factor.     

High-Temperature Behavior of Indent and Creep-Nucleated Cracks in Vitreous-Bonded Alumina

Crack behavior was studied at elevated temperatures in a commercial vitreous-bonded alumina for two types of cracks: one introduced by indentation at room temperature and the other by the creep process. Indentation cracks with relatively small initial size grew progressively longer during creep before they became blunt and arrested; however, they continued to widen throughout the creep process. Larger indentation cracks under high stress condition continued to grow until failure. The evolution of creep-nucleated cracks was so fast that they were observed only in their arrested state. Once observed, their length remained essentially constant, but they did grow in width. The crack-opening displacement rates of both types of cracks were linearly related to the creep rate as predicted by fracture mechanics for stationary cracks. All but the specimens with the largest indentation crack exhibited flaw tolerance in that they failed by the coalescence of creep-nucleated cracks instead of the growth of a single crack. The results illustrate the crack behavior in the brittle-to-ductile transition regime for ceramics that deform by grain boundary sliding.     

Strengthening of Vickers indented 3Y-TZP by hydrothermal ageing

The effect of hydrothermal ageing on indentation cracks has been determined in 3Y-TZP by measuring the flexure strength of indented specimens before and after ageing. A substantial increase in strength was observed after ageing, in contrast to the well known decrease in strength in smooth specimens with only natural flaws. The increase in strength with ageing also occurs if the indentation residual stresses are previously removed by annealing. Observations around the crack tip show the formation of a highly microcracked zone during vapour exposure. Fractographic and micro-Raman analysis observations show that the profile of the cracks is marked on the fracture surface by this zone which is intergranular with a crumbled appearance and in which transformation has taken place. The increase in strength is discussed in terms of crack tip blunting induced by the multiaxial stresses that develop in front of the crack under bending.     

Creep-Crack Growth by Damage Accumulation in a Glass-Ceramic

The growth rate, near-tip creep response, and damage processes of creep cracks in a pyroceram glass-ceramic were studied under tensile loading at elevated temperatures. The rates of crack extension were characterized as a function of the applied stress intensity factor. The damage processes which occurred near the crack tip and led to creep crack extension were identified using a replica technique and by direct observations in a scanning electron microscope equipped with a high-temperature loading stage. The accumulated creep strains near the crack tip were measured via the stereoimaging technique. The results indicate that creep-crack growth in the pyroceram glass-ceramic occurs in both continuous and discontinuous manners, with the damage processes manifested as the nucleation, growth, and coalescence of inhomogeneously distributed cavities and microcracks. Measurements of the total accumulated creep strain near the crack tip suggest that crack extension follows a critical strain criterion. Both the microcrack density and the total accumulated creep strain show similar dependence with distance from the crack tip. These observations suggest that damage accumulation and crack extension in the glass-ceramic are controlled by the near-tip creep rates.     

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.     

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.     

Effect of Microstructure on the Creep of Siliconized Silicon Carbide

Mechanisms of creep deformation have been investigated for a commercial grade of siliconized carbide containing ≅33%/silicon. Microstructural studies of both tensile and compressive test specimens indicate dislocation damage generation in both the silicon carbide and the silicon phases as a consequence of creep. In the silicon carbide, dislocation damage was normally restricted to contact sites between the silicon carbide grains resulting from high intergranular contact stresses during deformation. Dislocation damage was also observed in the silicon. Although dislocation damage was heavy in some regions of the specimens, most regions of the specimens, most regions were free of dislocations. This result is consistent with the hypothesis that deformations occurs by the motion of clusters of grains during deformation. In tension, creep at high strain rates, 1 × 10⁻⁸_S⁻¹, was accompanied by the formation of cavities at Si/SiC interfaces within the intergranular silicon phase. As cavities were not associated with dislocations, their growth was probably controlled by diffusional processes. Based on observations of the microstructure, a model of deformation is proposed to explain the fact that siliconized silicon carbide creeps faster in tension than in compression, at the same applied stress. The model is based on soil mechanics concepts. It is suggested that creep is controlled by intergranular friction between aggregate particles of the composite.     

Comparison of the Creep and Creep Rupture Performance of Two HIPed Silicon Nitride Ceramics

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 1260° and 1370°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.     

Diffusional Creep and Cavitational Strains in High-Purity Alumina under Tension and Subsequent Hydrostatic Compression

Diffusional creep and cavitation in pure alumina prepared with three different fabrication processes are compared under tension and subsequent hydrostatic compression. The deformation rates are separated into a volume-conserving creep rate and cavitational rate by measuring the longitudinal and transverse strains intermittently during deformation. Concurrent grain growth causes the volume-conserving strain rate to decrease in a manner consistent with Nabarro-Herring creep. The creep stress index of n = 1.3 and the average activation energy of Q = 480 kJ/mol are also consistent with Nabarro-Herring creep controlled by aluminum lattice diffusion. Anelastic loading and unloading transients are also identified and separated from the creep strains. High-voltage electron microscopy indicates that cavities nucleate at grain edges early and continuously in the creep process. The surfaces of these cavities tend after some growth to exhibit negligible curvature and various dihedral angles. The activation energy of Q = 450 kJ/mol and stress dependence of the cavitation rate of n = 1.3 are consistent with a grain boundary diffusional growth mechanism. The loading mode is found to have no significant effect on the cavitation rate during tensile creep and the subsequent decavitation rate during hydrostatic compression. The cavitation and decavitation rates are in good agreement with the model proposed by Speight and Beere when the effects of grain growth on cavity accumulation on grain boundaries are included. Exaggerated grain growth in high-density specimens can lead to early cavity coalescence and failure.     

High temperature slow crack growth in polyoxymethylene

Brittle failure has been observed in polyoxymethylene during long‐term low‐level tensile loading at elevated temperatures. It is argued to be associated with slow crack growth via the breakdown of the localized planar fibrillar damage zones that form under these conditions. This phenomenon has been characterized using notched compact tension specimens tested under various static loads and at different temperatures. The specimen lifetime at a given load is found to decrease strongly with increasing temperature and to increase with molar mass at a given load and temperature. The associated crack‐tip fibrillar damage zones are shown to arise from the breakdown of more localized microfibrillar deformation zones, which in turn result from interlamellar cavitation in the early stages of tensile deformation.     

Evolution of Stress Failure Resulting from High-Temperature Stress-Corrosion Cracking in a Hot Isostatically Pressed Silicon Nitride

Stress-corrosion cracking in a commercially available, hot isostatically pressed (HIPed), yttria-fluxed, silicon nitride was the prevalent mode of failure in specimens creepruptured at 1370°C. High-temperature diffusional processes associated with oxygen were responsible for the creation of an advancing stress-corrosion front that had formed at the specimen surface and advanced radially inward. The volume of material in the wake of the stress-corrosion front possessed a high concentration of lenticular cavities at two-grain boundaries, a high concentration of multigrain junction cavities, and large amorphous "pockets" in other multigrain junctions that were abnormally rich in oxygen and yttrium. The combination of tensile stress and the high concentration of cavities in the near-surface volume of the material resulted in microcrack coalescence or the formation of a planar, stress-corrosion crack . The concurrent growth of the stress-corrosion front and crack during the tensile creep-rupture tests ultimately led to stress-induced failure.     

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.     

Rising Fracture Toughness from the Bending Strength of Indented Alumina Beams

The analytical function of crack extension to a fractional power is used to represent the fracture resistance of a vitreous-bonded 96% alumina ceramic. A varying flaw size, controlled by Vickers indentation loading between 3 and 300 N, was placed on the prospective tensile surfaces of four-point bend specimens, previously polished and annealed. The lengths of surface cracks were measured by optical microscopy. Straight lines were fitted to the logarithmic functions of observed bending strength versus indentation load in two series of experiments: (I) including the residual stress due to indentation and (II) having the residual stress annealed out at an elevated temperature. Within the precision of measurement these lines have the same slope, being about 32% less than the -1/3 slope which a fracture toughness independent of crack extension would indicate. Considering the criteria for crack extension and specimen failure, the fracture mechanics equations were solved for the conditions of the two series of experiments. Approximately the same values of fracture toughness, rising as a function of indentation flaw size, were obtained from both series of experiments.