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.     

High-Temperature Tensile Behavior of a Boron Nitride-Coated Silicon Carbide-Fiber Glass-Ceramic Composite

Tensile properties of a cross-ply glass-ceramic composite were investigated by conducting fracture, creep, and fatigue experiments at both room temperature and high temperatures in air. The composite consisted of a barium magnesium aluminosilicate (BMAS) glass-ceramic matrix reinforced with SiC fibers with a SiC/BN coating. The material exhibited retention of most tensile properties up to 1200°C. Monotonic tensile fracture tests produced ultimate strengths of 230–300 MPa with failure strains of ∼1%, and no degradation in ultimate strength was observed at 1100° and 1200°C. In creep experiments at 1100°C, nominal steady-state creep rates in the 10⁻⁹ s⁻¹ range were established after a period of transient creep. Tensile stress rupture experiments at 1100° and 1200°C lasted longer than one year at stress levels above the corresponding proportional limit stresses for those temperatures. Tensile fatigue experiments were conducted in which the maximum applied stress was slightly greater than the proportional limit stress of the matrix, and, in these experiments, the composite survived 10⁵ cycles without fracture at temperatures up to 1200°C. Microscopic damage mechanisms were investigated by TEM, and microstructural observations of tested samples were correlated with the mechanical response. The SiC/ BN fiber coatings effectively inhibited diffusion and reaction at the interface during high-temperature testing. The BN layer also provided a weak interfacial bond that resulted in damage-tolerant fracture behavior. However, oxidation of near-surface SiC fibers occurred during prolonged exposure at high temperatures, and limited oxidation at fiber interfaces was observed when samples were dynamically loaded above the proportional limit stress, creating micro-cracks along which oxygen could diffuse into the interior of the composite.     

High-Temperature Fatigue Behavior of Polycrystalline Alumina

The strength and fatigue behavior of a 99.5% polycrystalline alumina were measured as a function of temperature. Both the strength and fatigue behavior remained essentially constant up to 500°C; from 800° to 1100°C the strength and fatigue resistance decreased markedly and at >1100°C macroscopic creep was observed. It is believed that the decrease in strength and fatigue resistance is caused by a grain-boundary glassy phase enhancing subcritical crack growth. Proof-testing at room temperature was effective in improving the strength distributions at both room temperature and 1000°C; however, at 1000°C it was not effective, due to crack growth during the proof test. The good agreement between proof-test results and fracture-mechanics theory indicates that the same flaws control the strength at room temperature and at high temperatures.     

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.     

Flexural Creep of Coated SiC-Fiber-Reinforced Glass-Ceramic Composites

This study reports the flexural creep behavior of a fiber-reinforced glass-ceramic and associated changes in micro-structure. SiC fibers were coated with a dual layer of SiC/BN to provide a weak interface that was stable at high temperatures. Flexural creep, creep-rupture, and creep-strain recovery experiments were conducted on composite material and barium-magnesium aluminosilicate matrix from 1000° to 1200°C. Below 1130°C, creep rates were extremely low (∼10⁻⁹ S⁻¹), preventing accurate measurement of the stress dependence. Above 1130°C, creep rates were in the 10⁻⁸ s⁻¹ range. The creep-rupture strength of the composite at 1100°C was about 75–80% of the fast fracture strength. Creep-strain recovery experiments showed recovery of up to 90% under prolonged unloading. Experimental creep results from the composite and the matrix were compared, and microstructural observations by TEM were employed to assess the effectiveness of the fiber coatings and to determine the mechanism(s) of creep deformation and damage.     

Cyclic-Fatigue Behavior of SiC/SiC Composites at Room and High Temperatures

Tension-tension cyclic-fatigue tests of a two-dimensional-woven-SiC-fiber-SiC-matrix composite (SiC/SiC) prepared by chemical vapor infiltration (CVI) were conducted in air at room temperature and in argon at 1000°C. The cyclic-fatigue limit (10⁷ cycles) at room temperature was ∼160 MPa, which was ∼80% of the monotonic tensile strength of the composite. However, the fatigue limit at 1000°C was only 75 MPa, which was 30% of the tensile strength of the composite. No difference was observed in cyclic-fatigue life at room temperature and at 1000°C at stresses >180 MPa; however, cyclic-fatigue life decreased at 1000°C at stresses < 180 MPa. The fracture mode changed from fracture in 0° and 90° bundles at high stresses to fracture mainly in 0° bundles at low stresses. Fiber-pullout length at 1000°C was longer than that at room temperature, and, in cyclic fatigue, it was longer than that in monotonic tension. The decrease in the fatigue limit at 1000°C was concluded to be possibly attributed to creep of fibers and the reduction of the sliding resistance of the interface between the matrix and the fibers.     

Stress Rate Dependence of Fracture Strength in Pre-Cracked Silicon Nitride Ceramics Doped with Ytterbium Oxide

High-temperature dynamic fatigue behavior has been investigated in 6 wt% ytterbium oxide and 2 wt% alumina-doped silicon nitride ceramics by nitrogen gas pressure sintering. The specimens were pre-cracked by Vickers indentation to prevent creep damage and to ensure dynamic fatigue dominating. The tests were performed in four-point flexure in air at temperatures of 1000°, 1200°, 1300°, and 1400°C and by varying the loading rate from 1, 0.5, 0.1–0.01 mm/min at each temperature. The analyses were conducted by plotting fatigue stress against loading rate at each testing temperature in double logarithm coordinates. The material was found to be the least susceptible (the highest slow crack exponent number N ) to slow crack growth at 1200°C, as reflected by the comparison of the plot slopes for the four testing temperatures. The explanation and analyses take into consideration the grain-boundary phase crystallization, crack healing, and oxidation during testing evidenced by X-ray diffraction and transmission electron microscopy. The fracture surfaces were characterized by three well-defined zones, namely zone I, II, and III, referring to the pre-cracked area, slow crack growth area, and fast fracture area, respectively.     

Fracture and Crack Healing in (U,Pu)C

The fracture stress of several types of (U,Pu)C_1+x pellets was measured from 25° to 1200°C at a fixed strain rate. The fracture stress increases with temperature and the fracture is predominantly transgranular up to ≊500°C. At >500°C, the fracture stress decreases as the temperature increases and the fracture becomes increasingly intergranular. The flow stress, σ_0.002, decreased rapidly between 1000° and 1600°C. An investigation of the stress dependence and kinetics of crack healing at 1300° to 1600°C indicates that strength may recover by a volume-diffusion-controlled mechanism.     

Accumulation of Creep Damage in a Siliconized Silicon Carbide

The accumulation of creep damage in a siliconized silicon carbide was investigated as a function of applied stress, creep strain, and microstructure. At 1100°C, creep damage was observed to accompany deformation in specimens tested to creep strains greater than 0.10%, under applied stresses greater than 137 MPa. At low creep strains, creep damage occurred in regions of the microstructure of high silicon carbide content. As deformation progressed, creep damage extended into regions of the microstructure of lower silicon carbide content. The area density and area fraction of cavities were found to increase linearly with creep strain. From these results, a threshold stress for the formation of creep damage was determined to be 132 MPa at 1100°C. It was suggested that the formation of creep damage was controlled by the heterogeneous nucleation of cavities at the silicon-silicon carbide interface, with the aid of high localized stresses and iron impurities in the silicon phase.     

Tensile Creep and Creep-Strain Recovery Behavior of Silicon Carbide Fiber/Calcium Aluminosilicate Matrix Ceramic Composites

The tensile creep and creep strain recovery behavior of 0° and 0°/90° Nicalon-fiber/calcium aluminosilicate matrix composites was investigated at 1200°C in high-purity argon. For the 0° composite, the 100-h creep rate ranged from approximately 4.6 × 10⁻⁹ s⁻¹ at 60 MPa to 2.2 × 10⁻⁸ s⁻¹ at 200 MPa. At 60 MPa, the creep rate of the 0°/90° composite was approximately the same as that found for the 0° composite, even though the 0°/90° composite had only one-half the number of fibers in the loading direction. Upon unloading, the composites exhibited viscous strain recovery. For a loading history involving 100 h of creep at 60 MPa, followed by 100 h of recovery at 2 MPa, approximately 27% of the prior creep strain was recovered for the 0° composite and 49% for the 0°/90° composite. At low stresses (60 and 120 MPa), cavities formed in the matrix, but there was no significant fiber or matrix damage. For moderate stresses (200 MPa), periodic fiber rupture occurred. At high stresses (250 MPa), matrix fracture and rupture of the highly stressed bridging fibers limited the creep life to under 70 min.     

Crack-Healing Behavior of Si3N4/SiC Ceramics under Cyclic Stress and Resultant Fatigue Strength at the Healing Temperature

Si₃N₄/SiC composite ceramics were sintered and subjected to three-point bending. A semi-elliptical surface crack of 100 μm surface length was made on each specimen. The crack-healing behavior under cyclic stress of 5 Hz, and resultant cyclic fatigue strengths at healing temperatures of 1100° and 1200°C, were systematically investigated. The main conclusions are as follows: (1) Si₃N₄/SiC composite ceramics have an excellent ability to heal a crack at 1100° and 1200°C. (2) This sample could heal a crack even under cyclic stress at a frequency of 5 Hz. (3) The crack-healed sample exhibited quite high cyclic fatigue strength at each crack-healing temperature, 1100° and 1200°C.     

Mechanical Properties of Magnesia Single Crystals Corn pression

Stress-strain curves of single crystals of magnesia compressed in the [100] direction are reported at temperatures from –196° to 1200°C.; curves are also shown for different rates of loading at room temperature. The crystals show considerable ductility at all temperatures and at room temperature can be deformed plastically about 6% before fracture at stresses which are about one-quarter of reported polycrystalline fracture strengths. The macroscopic yield drops apparently exponentially from an extrapolated value of 50,000 lb. per sq. in. at absolute zero to about 4500 lb. per sq. in. at temperatures of 900°C. and higher. Heat-treatment has an appreciable effect on the yield stress. The resistance of the material to deformation increases with the number of slip systems and bands activated because of the barriers to dislocation movements which occur at slip band intersections. At about 2 to 3% strain, stress concentrations begin to be relieved by small internal cracks which are not easily propagated. This effect is extensive before final macroscopic failure of the crystal occurs. Preliminary creep tests above the macroscopic yield stress and in the temperature range 800° to 1000°C. show large instantaneous plastic deformations followed by slow constant-rate creep.     

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.     

Crack Healing and Bending Strength of Aluminum Titanate Ceramics at High Temperature

Bending strength and Young's modulus of aluminum titanate ceramics at room temperature to 1300°C were examined. Bending strength increased from 62 MPa at room temperature to 280 MPa at 1100°C. Young's modulus also increased, to 99 GPa at 1100°C. These increments were caused by crack healing. In particular, crack cylinderization occurring at 1000° to 1100°C markedly increased the mechanical strength. The thermal-hysteresis curves also showed healing of grain-boundary cracks.     

Effectiveness of Monazite Coatings in Oxide/Oxide Composites after Long-Term Exposure at High Temperature

The effectiveness of monazite (LaPO₄) in providing an oxidation-resistant weak fiber/matrix interface was evaluated in a fiber roving/thin coating/ceramic-matrix composite with >20% fiber volume fraction. Nextel™ 610/monazite/alumina composites were fabricated and tensile tested after isothermal exposures of up to 1000 h. Some strength loss was seen after short-term exposures (1100°–1200°C/5–250 h); however, no further loss was observed after 1000 h at 1200°C. Conversely, control samples containing uncoated fiber displayed >70% strength losses after only 5 h at 1200°C. Fiber pullout was seen in monazite-containing samples even after 1000 h at 1200°C. Debonding was predominantly in the coating or at either the fiber/coating or coating/matrix interface. Push-out testing confirmed the weakness of the monazite coating interface.     

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.     

Effect of Heat Treatments on the Crack-Healing and Static Fatigue Behavior of Silicon Carbide Sintered with Sc2O3 and AlN

Crack-healing behavior of silicon carbide ceramics sintered with AlN and Sc₂O₃ has been studied as a function of heat-treatment temperature and applied stress. Results showed that heat treatment in air could significantly increase the indentation strength whether a stress is applied or not. After heat treatment with no applied stress at 1300°C for 1 h in air, the indentation strength of the specimen with an indentation crack of ∼100 μm (≈2c) recovered its strength fully at room temperature. In addition, a simple heat treatment at 1200°C for 5 h under an applied stress of 200 MPa in air resulted in a complete recovery of the unindented strength at the healing temperature. However, higher applied stress led to fracture of the specimens during heat treatment. The static fatigue limit of the specimens crack healed at 1200°C for 5 h under 200 MPa was ∼450 MPa at the healing temperature. The ratio of the static fatigue limit of the crack-healed specimen to the unindented strength was ∼80%.     

Temperature-dependent mechanical and long crack behavior of zirconium diboride–silicon carbide composite

Hot pressed ZrB2–20 vol.% SiC ultra-high temperature ceramic composites have been prepared for strength and fracture investigations. Two composites fabricated under differing hot pressing temperatures with (ZSB) and without (ZS) B4C sintering aids were selected for room temperature modulus of rupture (MOR) strength and single-edge-notch bend (SENB) fracture toughness experiments. Structure property relationships were examined for both composites. MOR and stiffness temperature dependence was also investigated up to 1500 °C. Long crack propagation studies were conducted up to 1400 °C using the double cantilevered beam geometry with half-chevron-notch initiation zones. Residual Boron-rich carbide maximum particle sizes were found to be strength limiting in ZSB billets while SiC controlled strength in ZS billets. Flexure strength decreased linearly with temperature from 1000 to 1500 °C with no visible plastic deformation prior to fracture. Similar stiffness decreases were observed with a transition temperature range of 1100–1200 °C. Long crack studies produced R-curves that show no significant toughening behavior at room temperature with some modest rising R-curve behavior appearing at higher temperatures. These studies also show the plateau toughness increases with temperature up to 1200 °C. This is supported by an observed transition from primarily transgranular fracture at room temperature to primarily intergranular fracture at high temperatures. Wake zone toughening is evident up to 1000 °C with K_R rise from 0.1 to 0.5 MPa√m. Beyond 1000 °C fracture mechanism transitions to include creep zone development ahead of crack tip with wake zone toughening vanishing.     

Stress Relaxation of Compression Loaded Plasma-Sprayed 7 Wt% Y2O3–ZrO2 Stand-Alone Coatings

Stand-alone plasma-sprayed tubes of 7 wt% Y₂O₃–ZrO₂ made from the same starting powder but at two different sites were subject to stress-relaxation testing in axial compression at temperatures of 25°, 1000°, 1050°, 1100°, and 1200°C and at an initial stress of 10–80 MPa. A time-dependent stress response was observed for both coatings at all temperatures. For example, a 20 MPa stress applied at 1050°C relaxed to ∼3 MPa in 180 min. When the same initial stress was applied at 1200°C, the coating fully relaxed in 32 min. For all experimental conditions evaluated, an initial fast stress-relaxation regime was observed (<10 min), followed by a slower second stress-relaxation regime at later times (>10 min). Coatings with higher as-sprayed densities exhibited a lengthened fast relaxation regime as compared with less dense coatings. A Maxwell model was modified in order to provide an accurate fit to the experimental stress-relaxation curves. From scanning electron microscopy experiments and mechanical data, the mechanism for stress relaxation from 25°C through 1200°C, particularly during fast relaxation, was proposed to be the formation of cracks parallel with respect to the applied load. In addition to this mechanism, stress relaxation that occurred in specimens tested at 1000°C through 1200°C was proposed to be due to partial or complete closure of cracks oriented perpendicular to the applied stress.     

Structural Reliability of Yttria-Doped Hot-Pressed Silicon Nitride at Elevated Temperatures

The strength of yttria-doped hot-pressed silicon nitride was investigated as a function of temperature, time, and applied load. Data collected at 1200°C are presented in the form of a strength-degradation diagram for an applied stress of 350 MPa. At this temperature, the behavior of yttria-doped hot-pressed silicon nitride is found to be superior to that of magnesia-doped hot-pressed silicon nitride, in which creep results in the formation of microcracks that lead to strength degradation. By contrast, the yttria-doped material does not suffer from microcrack formation or strength degradation at 1200°C. Strength degradation does occur at higher temperatures and, as a consequence, an upper limit of 1200°C is recommended for yttria-doped hot-pressed silicon nitride in structural applications.