Creep Deformation in an Alumina–Silicon Carbide Composite Produced via a Directed Metal Oxidation Process

Flexural creep studies were conducted in a commercially available alumina matrix composite reinforced with SiC particulates (SiC_p) and aluminum metal at temperatures from 1200° to 1300°C under selected stress levels in air. The alumina composite (5 to 10 μm alumina grain size) containing 48 vol% SiC particulates and 13 vol% aluminum alloy was fabricated via a directed metal oxidation process (DIMOX(tm))† and had an external 15 μm oxide coating. Creep results indicated that the DIMOX Al₂O₃–SiC_p composite exhibited creep rates that were comparable to alumina composites reinforced with 10 vol% (8 (μm grain size) and 50 vol% (1.5 μm grain size) SiC whiskers under the employed test conditions. The DIMOX Al₂O₃–SiC_p composite exhibited a stress exponent of 2 at 1200°C and a higher exponent value (2.6) at ≥ 1260°C, which is associated with the enhanced creep cavitation. The creep mechanism in the DIMOX alumina composite was attributed to grain boundary sliding accommodated by diffusional processes. Creep damage observed in the DIMOX Al₂O₃-SiC_p composite resulted from the cavitation at alumina two-grain facets and multiple-grain junctions where aluminum alloy was present.     

Atmospheric Effects on Compressive Creep of SiC-Whisker-Reinforced Alumina

A SiC-whisker-reinforced alumina composite was crept in compression at 1200° to 1400°C in an air ambient and in nitrogen. The data were described by a power-law-type constitutive relation. The measured value of the stress exponent was n = 1 at 1200°C and n = 3 at 1300° and 1400°C in both ambients. TEM observations were correlated with the measured creep response to determine active deformation mechanisms. Values of n = 1 were associated with diffusional creep and unaccommodated grain-boundary sliding, while values of n = 3 were associated with increased microstructural damage in the form of cavities. Experiments conducted in circulated air resulted in higher creep rates than comparable experiments in nitrogen. The accelerated creep rates were caused by the thermal oxidation of SiC and the resultant formation of a vitreous phase along composite interfaces. The glassy phase facilitated cavitation, weakened interfaces, and enhanced boundary diffusion.     

Tensile Creep Behavior of Alumina/Silicon Carbide Nanocomposite

Tensile creep and creep rupture behaviors of alumina/17 vol% silicon carbide nanocomposite and monolithic alumina Were investigated at 1200° to 1300°C and at 50 to 150 MPa. Compared to the monolithic alumina, the nanocomposite exhibited excellent creep resistance. The minimum creep rate of the nanocomposite was about three orders of magnitude lower and the creep life was 10 times longer than those of the monolith. The nanocomposite demonstrated transient creep until failure, while accelerated creep was observed in the monolith. It was revealed that rotating and plunging of intergranular silicon carbide nanoparticles into the alumina matrix increased the creep resistance with grain boundary sliding.     

High-Temperature Creep Deformation of Alumina — SiC-Whisker Composites

The creep resistance at temperatures between 1200° and 1300°C in air of alumina—SiC-whisker composites was investigated via four-point flexure to examine (1) the effect of whisker content and (2) the influence of densification additives (i.e., Y₂O₃ (plus MgO)). The creep resistance of polycrystalline alumina is greatly improved with the addition of ≤ 20 vol% SiC whiskers. The interlocking/pinning of grains by whiskers which limits grain-boundary sliding contributes to the improvement in creep resistance. However, the creep rates of alumina composites in air increase at whisker contents ≥ 30 vol%. Electron microscopy observations suggested that the degradation in creep resistance for whisker content ≥ 30 vol% originated from (1) the promotion of creep cavitation and subsequent microcrack generation from the higher number density of nucleation sites and (2) more extensive formation of grain-boundary amorphous phase(s) associated with an observed increased oxidation rate. Along this one, the excellent creep resistance of alumina composites containing 20 vol% SiC whiskers was significantly degraded by the presence of the intergranular amorphous phases introduced by the addition of the Y₂O₃ densification additive.     

Effect of Yttria and Yttrium-Aluminum Garnet on Densification and Grain Growth of Alumina At 1200°–1300°C

Densification and grain growth of alumina were studied with yttria or yttrium-aluminum garnet (YAG) additives at the relatively low temperatures of 1200°–1300°C. Yttria doping was found to inhibit densification and grain growth of alumina at 1200°C and, depending on dopant level, had a lesser effect at 1300°C. At 1200°C, yttria inhibits densification more than it hinders grain growth. The rate of grain growth increases faster with temperature than the rate of densification. Alumina-YAG particulate composites were difficult to sinter, yielding relative densities of only 65% and 72% after 100 h at 1200° and 1300°C, respectively. Pure YAG compacts exhibited essentially no densification for times up to 100 h at 1300°C.     

Deformation Mechanism of Fine-Grained Magnesium Aluminate Spinel Prepared Using an Alkoxide Precursor

Polycrystalline MgAl₂O₄ spinel with high purity and stoichiometric composition was prepared using alkoxide precursors. The average grain size of the polycrystal was fine (1.7 μm). The deformation mechanism of the polycrystal was investigated in air at temperatures of 1300°–1400°C. At 1300°C, oxygen lattice diffusion controlled the deformation, despite the fine grain size; however, increases in the temperature and applied stress caused cavities to nucleate and grow. Spinel possessed better creep resistance than alumina of comparative grain size. The effective diffusion coefficient was determined as follows: [formula omitted]     

Creep behaviour of alumina–mullite–zirconia nanocomposites obtained by a colloidal processing route

The high-temperature creep behaviour of high-purity alumina (A) and an alumina–mullite–zirconia nanocomposite (AZS) has been studied. The alumina–mullite–zirconia nanocomposite was prepared by using a colloidal processing route (powder–alkoxide mixtures). Creep tests were carried out in air in a 4-point-bending-fixture from 1200 to 1400 °C under constant stresses ranging from 30 to 220 MPa. Creep parameters (stress exponent n and activation energy Q) were correlated with microstructural features in order to determine the dominant creep mechanisms for both materials. The slow crack growth region (SCG), given by pairs of critical stress and the corresponding critical strain rate at the temperatures 1200, 1300 and 1400 °C of both materials was studied.

It was found that the creep rate of AZS was two orders of magnitude lower than the creep rate of undoped alumina A. The dominant creep mechanism of A is assumed to be a combination of grain boundary and lattice diffusion controlled creep. The creep mechanism for AZS is different and depends on the temperature. It is supposed that lattice diffusion controlled creep (Nabarro–Herring) is the dominant creep mechanism at 1200 °C, whereas at 1300 °C it is supposed to be grain boundary sliding accommodated by grain boundary diffusion. Comparing the slow crack growth region of both materials, a dramatic improvement was observed. The slow crack growth region of alumina is shifted nearly twice concerning the applied stresses for AZS at the temperatures 1200, 1300 and 1400 °C.     

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 of MgO Containing a Dispersion of Carbon

Creep experiments on polycrystalline MgO containing a fine dispersion of carbon are reported. The samples were prepared by hot-pressing and creep was measured in four-point bending under stresses of 1000 to 5000 psi at 1000° to 1300° C. Although results for MgO creep without carbon addition are in good agreement with published reports, introducing dispersions of 0.5 to 2 vol% C into MgO modifies its creep behavior. Comparing specimens of the same grain size, the samples containing the carbon dispersion had lower creep rates than those of MgO without addition. This effect increased with increasing carbon additions. The stress exponent remained small (1 to 2) in all cases. The apparent activation energy for creep increased dramatically with the carbon additions. Possible mechanisms for the influence of this dispersion on creep are discussed briefly.     

Flexural Creep Deformation of ZrB2/SiC Ceramics in Oxidizing Atmosphere

Flexural creep of ZrB₂/0–50 vol% SiC ceramics was characterized in oxidizing atmosphere as a function of temperature (1200°–1500°C), stress (30–180 MPa), and SiC particle size (2 and 10 μm). Creep behavior showed strong dependence on SiC content and particle size, temperature and stress. The rate of creep increased with increasing SiC content, temperature, and stress and with decreasing SiC particle size, especially, at temperatures above 1300°C. The activation energy of creep showed linear dependence on the SiC content increasing from about 130 to 511 kJ/mol for ceramics containing 0 and 50 vol% 2-μm SiC, respectively. The stress exponent was about 2 for ZrB₂ containing 50 vol% SiC regardless of SiC particle size, which is an indication that the leading mechanism of creep for this composition is sliding of grain boundaries. Compared with that, the stress exponent is about 1 for ZrB₂ containing 0–25vol% SiC, which is an indication that diffusional creep has a significant contribution to the mechanism of creep for these compositions. Cracking and grain shifting were observed on the tensile side of the samples containing 25 and 50 vol% SiC. Cracks propagate through the SiC phase confirming the assumption that grain-boundary sliding of the SiC grains is the controlling creep mechanism in the ceramics containing 50 vol% SiC. The presence of stress, both compressive and tensile, in the samples enhanced oxidation.     

Effect of Processing on Microstructure and Mechanical Behavior of Magnesium Oxide

Polycrystalline MgO specimens were fabricated from two powders by hot-pressing in graphite or alumina dies and annealing in air, in vacuum, or within the graphite die in vacuum. Parameters affected were density, grain size, and visual appearance, which was considered to be dependent on grain boundary structure. The formation of a boundary liquid phase with one type of powder tended to eliminate the effect of the processing variables. The character (microstructure) of the specimens was correlated with their mechanical behavior in compression at a constant strain rate at 1200°C.     

Microstructural evolution under load and high temperature deformation mechanisms of a mullite/alumina fibre

A two-phase mullite alumina fibre, the 3M Nextel 720 fibre, has been studied in tension and creep. The fibre shows the highest creep resistance of all current commercial fine oxide fibres up to 1500 °C. The creep mechanisms involve progressive dissolution of mullite and simultaneous reprecipitation of alumina into elongated oriented grains and grain boundary sliding by a thin alumino-silicate liquid phase. The rate of grain growth in creep at a given temperature is dependant on the applied stress. The combination of sub-micron size mullite crystallites and alumina grains gives rise to a high sensitivity to alkaline contamination. Stress enhanced diffusion of the contaminants from the fibre surface results in crack nucleation, dissolution of mullite, formation of a liquid phase and slow crack growth. From 1200 °C, this process is coupled with a fast α-alumina grain growth at the fibre surface.     

Creep Behavior of a SiC-Whisker-Reinforced Alumina

Creep tests in four-point flexure loading configuration in air employing applied stresses of 37 to 300 MPa at temperatures of 1200°, 1300°, and 1400°C were performed on 20-vol%-SiC-whisker-reinforced alumina and unreinforced single-phase polycrystalline alumina. The creep rate of polycrystalline alumina was significantly reduced through the addition of SiC whiskers, although strain to failure was lower. Transmission and scanning electron microscopy results suggest that substantial increase in the creep resistance in flexure of alumina composites originates from the retardation of grain-boundary sliding by the SiC whiskers.     

Synthesis, Characterization, and Consolidation of Si3N4 Obtained from Ammonolysis of SiCl4

Thermal decomposition of silicon diimide, Si(NH)₂, in vacuum resulted in very-high-purity, fine-particle-size, amorphous Si₃N₄ powders. The amorphous powder was isothermally aged at 50° to 100° intervals from 1000° to 1500°C for phase identification. Examination of ir spectra and X-ray diffraction patterns indicated a slow and gradual transition from an amorphous material to a crystalline α-phase occurring at 1200°C for >4 h and/or 1300° to 1400°C for 2 h. As the temperature was increased to ≥1450°C for 2 h, the crystalline β-phase was observed. Phase nucleation and crystallite morphology in this system were studied by electron microscopy and electron diffraction combined with TG as functions of temperature for the inorganic polymer starting materials. Powders prepared in this manner with 4 wt% Mg₃N₂ added as a sintering aid were hot-pressed to high-density fine-grained bodies with uniform microstructures. The optimum hot-pressing condition was 1650°C for 1 h. Silicon concentration steadily increased as the hot-pressing temperature or time was increased. A method for chemical etching for high-density fine-grained Si₃N₄ is described. Electrical measurements between room temperature and ∼500°C indicated dielectric constant and tan δ values of 8.3±0.03 and 0.65±0.05×10⁻², respectively.     

Thermal stress relaxation creep and microstructural evolutions of nanostructured SiC ceramics by liquid phase sintering

We explored the thermal relaxation creep characteristics of nanostructured SiC ceramics by bend stress relaxation (BSR) method. The effects of the differences in microstructure and secondary phases by liquid phase sintering at 1800 or 1900 °C were especially discussed, based on microstructural evolutions during the creep. The creep was characterized by the BSR ratio (m) of ～0.80 up to 1200 °C, and the proportion of amorphous phase as a secondary phase was related to the creep resistance at 1300 °C. The microstructural evolutions during the creep consisted firstly in the re-distribution of amorphous phase, probably as a consequence of its viscous flow, and secondly in an extensive nucleation and growth of cavities. Furthermore, the former enhanced inter-diffusion of Al–Y among intergranular areas above the ternary eutectic temperature, which caused the significantly reduced creep resistance, and the latter reflected the crystalline YAG decomposition as another secondary phase near 1500 °C.     

Experimental Assessment of Plasticity of Nanocrystalline 1.7 mol% Yttria Tetragonal Zirconia Polycrystals

High temperature mechanical behavior of nanocrystalline 1.7 mol% (3 wt%) yttria tetragonal zirconia polycrystals (nc-YTZP) was characterized by compression creep tests. The hot isostatically pressed nc-YTZP with mean grain size of 120 nm was subjected to grain growth to obtain grain sizes in the range of 120–310 nm. Direct measurements of the creep parameters were performed in the temperature range 1150°–1300°C and stress range 5–400 MPa. The strain rates at 1150°C ranged between 2 × 10⁻⁷ and 9 × 10⁻⁵ s⁻¹ when increasing the stress from 15 to 400 MPa. Values of the stress exponent, n =2.0±0.3, and the activation energy, Q =630±40 kJ/mol, were obtained for all test conditions. A value of the grain size exponent, p =1.5±0.3, was obtained at 1150°C in the stress range studied. Detailed microstructural observations revealed the absence of glassy phase at the grain boundaries. The creep parameters were compared with those from the literature, and the results were discussed in terms of the model recently developed by the authors, with a reasonable agreement.     

Effect of Thermal Exposures on the Strengths of Nextel™ 550 and 720 Filaments

The effects of thermal exposure on the strengths of Nextel™ 550 and 720 tows, bare and coated with carbon, were determined by room-temperature tensile testing of single filaments extracted from tows that had been exposed to different thermal environments (i.e., air or vacuum) at temperatures from 550° to 1400°C. The results help define the allowable composite processing conditions when using these tows. A 28% drop in the strength of Nextel 550 filaments occurred after a thermal exposure at 1100°C for 2 h in air. After an exposure of 1300°C/2 h/air, a strength degradation of ∼47% resulted. Filaments exposed above 1100°C under vacuum showed more severe strength degradation than filaments exposed in air. The observed strength degradation may stem from a combination of phase transformations of the alumina, the onset of mullite crystallization, and/or exaggerated mullite grain growth. Strength after heat treatment under vacuum at 1050° and 1150°C did not deteriorate as rapidly as after heat treatment under vacuum between 950° and 1050°C or between 1150° and 1250°C. This may be a result of the competition between healing of flaws by the amorphous silica and its evaporation (leading to an increase in its viscosity or loss) and/or densification of the filaments. Nextel 720 filaments exhibited about 9% strength loss after an exposure at 1100°C/2 h/air. The filaments maintained 75% of their strength after a 1300°C/2 h/air heat treatment. The observed strength degradation may stem from thermal grooving, grain growth, and/or annealing of the mullite subgrain boundaries. Thermal exposure of >10 h at 1300°C was required to produce measurable grain growth. Strength loss between 1200° and 1300°C (air heat treatment) was not as great as between 1100° and 1200°C or 1300° and 1400°C.     

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.     

Influence of Amorphous Grain Boundary Phases on the Superplastic Behavior of 3-mol%-Yttria-Stabilized Tetragonal Zirconia Polycrystals (3Y-TZP)

Amorphous silicate grain boundary phases of varying chemistry and amounts were added to 3Y-TZP in order to determine their influence on the superplastic behavior between 1200° and 1300°C and on the room-temperature mechanical properties. Strain rate enhancement at high temperatures was observed in 3Y-TZP containing a glassy grain boundary phase, even with as little as 0.1 wt% glass. Strain rate enhancement was greatest in 3Y-TZP with 5 wt% glass, but the room-temperature hardness, elastic modulus, and fracture toughness were degraded. The addition of glassy grain boundary phases did not significantly affect the stress exponent of 3Y-TZP, but did lower the activation energy for superplastic flow. Strain rate enhancement was highest in samples containing the grain boundary phase with the highest solubility for Y₂O₃ and ZrO₂, but the strain rate did not scale inversely with the viscosity of the silicate phases. Grain boundary sliding accommodated by diffusional creep controlled by an interface reaction is proposed as the mechanism for superplastic deformation in 3Y-TZP with and without glassy grain boundary phases.     

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.