Compressive Creep of SiC-Whisker-Reinforced Al2O3

Compressive creep of SiC-whisker-reinforced Al₂O₃ composites (0, 5, 15, and 25 wt% SiC) was measured in the temperature range of 1300° to 1500°C in air and argon. The creep resistance increased with increasing whisker concentration. The results indicated that the whiskers degraded in air, increasing strain rates compared to those in argon. Stress exponents between 1.0 and 2.0 and an activation energy of 620 ± 100 kJ/mol were measured. Transmission electron microscopy observations indicated that cavitation was minimal and that the deformed composites had the same dislocation structure as did the as-received samples.     

SiC-Whisker-Reinforced Glass-Ceramic Composites: Interfaces and Properties

Different types of SiC whiskers were incorporated into lithium aluminosilicate (LAS) and calcium aluminosilicate (CAS) glass-ceramic matrices. Interfaces in these composites were characterized using Auger spectroscopy, scanning electron microscopy (SEM), and transmission electron microscopy (TEM), and the observations were correlated with measurements of fracture toughness and strength. The chemistry and morphology of the resulting interfaces affected the composite strength and toughness and controlled the mode of crack propagation. Certain types of SiC whiskers were characterized by a carbon-rich near-surface chemistry that became more carbon rich after composite fabrication. In these materials, the flexural strength at 20°C increased by up to 400% and the fracture toughness increased by up to 500%. Crack propagation modes were characterized by crack deflection, whisker–matrix debonding, and crack bridging. In contrast, SiC whiskers with stoichiometric near-surface chemistry generally did not form carbon-rich interfaces during composite fabrication, resulting in composites with low strength and fracture toughness.     

Mechanical Properties of Si2N2O/SiC-Whisker Composites

The mechanical and thermal properties of Si₂N₂O/SiC-whisker composites were studied with emphasis on the effect of matrix composition and of whisker content. The fracture toughness of Si₂N₂O was remarkably improved by 90% with a concomitant 70% strength improvement by addition of SiC whiskers of only 10 vol%. Optimum mechanical and thermal properties of Si₂N₂O/SiC-whisker composites were obtained at an equimolar ratio of Si₃N₄/SiO₂, which is the stoichiometric composition for Si₂N₂O. Additional investigation concerning the Si₂N₂O-matrix/SiC-whisker interface by controlling sintering additives is necessary for further improvement of mechanical and thermal properties of Si₂N₂O/SiC-whisker composites.     

Slip Casting of SiC-Whisker-Reinforced Si3N4

Si₃N₄ composite materials containing up to 20 vol% SiC whiskers were slip cast and pressureless sintered at 1820°C and 0.13 MPa of N₂. Viscosimetry showed no influence of whisker loading on the rheology of the highly concentrated aqueous slips up to 15 vol% whiskers. During casting the whiskers were preferentially aligned parallel to the mold surfaces. Depending on the whisker loading, green densities of 0.64 to 0.69 fractional density could be achieved. Strong anisotropic shrinkage occurred during sintering with a maximum linear shrinkage of 21% perpendicular but only 7% parallel to the whisker plane. With increasing whisker content from 0 to 20 vol% sintered densities decreased from 0.98 to 0.88, respectively.     

Si3N4/SiC-Whisker Composites without Sintering Aids: III, High-Temperature Behavior

The fracture behavior at high temperature of a Si₃N₄-based SiC-whisker composite fabricated by hot isostatic pressing without sintering aids is compared with that of other highly refractory materials. Particular attention is directed toward evaluating the slow-crack-growth resistance of the composite up to 1440°C and relating this resistance to the microfracture behavior of Si₃N₄ grains, SiC whiskers, and the intergranular, glassy SiO₂ phase. Only thick whiskers operate to bridge the wake of the crack; these whiskers may make a positive contribution to the slow-crack-growth resistance. Impurities detected by EDX microanalysis at the grain boundary, however, apparently degrade the high-temperature properties, a finding supported by internal-friction measurements. Nevertheless, the high potential of the system without sintering aids for high-temperature structural applications has been demonstrated by the time to failure estimated from the measured slow-crack-growth resistance for a fixed flaw size.     

Si3N4/SiC-Whisker Composites without Sintering Aids: II, Fracture Behavior

The fracture behavior of an Si₃N₄/SiC-whisker composite fabricated without sintering aids is investigated using a double approach based on the examination of R -curve behavior and a statistical analysis of crack propagation. In the composite with 20 vol% whisker, a 30% increase in toughness over the matrix value can be attributed to crack-tip phenomena. Strong interfacial bonding prevents any contribution to toughening by mechanisms operating in the wake region of the crack. Based on experimental observations of microfracture in both SiC whiskers and Si₃N₄ grains, toughening caused by crack-tip phenomena is quantitatively discussed in terms of fracture energy and whisker-distribution parameters.     

Elastic Properties of Al2O3 and Si3N4 Matrix Composites with SiC Whisker Reinforcement

A study of the elastic moduli of Al₂O₃ and Si₃N₄ ceramics reinforced with 0 to 25 wt% SiC whiskers has been performed. The Young's moduli, shear moduli, and longitudinal modulus are compared with calculated predictions for aligned fiber composites by Hill and Hashin and Rosen, and for fibers randomly oriented in three dimensions by Christensen and Waal. The measured values are in excellent quantitative agreement with those derived for the random orientation of the SiC whiskers.     

Analysis of Residual Stress in 6H-SiC Particles within Al2O3/SiC Composites through Raman Spectroscopy

We measured the Raman spectrum associated with the E₂-TO_quasi and LO_quasi modes of 6H-SiC particles as a function of hydrostatic pressure using a diamond anvil cell. The results of this calibration experiment were used to analyze the residual stress in 6H-SiC particles within Al₂O₃/SiC composites with 12%, 20%, and 30% SiC by volume. The Raman spectra show that residual stress in the SiC near the surface of the composites is −2040 ± 120, −1841 ± 110, and −1615 ± 100 MPa for the 12%, 20%, and 30% SiC composites, respectively. The measured decrease in stress with increasing packing fraction is consistent with theoretical predictions based on micromechanics.     

Microstructure and Densification of Pressureless-Sintered Al2O3/Si3N4-Whisker Composites

Composite densification was studied by performing slip casting and sintering experiments on an Al₂O₃ matrix and Si₃N₄ whisker system. Even though all the slip-cast powder compacts exhibited high green densities (up to 70% of the theoretical) and narrow pore-size distribution (pore radius around 15 to 30 nm), significant differential densification on a microscopic scale was found due to the existence of local whisker agglomeration. The inhomogeneous whisker distribution resulted in a binary mixture of large and small pores in the sintered composites, in which whisker-associated flaws remained stable even after prolonged sintering. The sintered microstructures showed that the spatial distribution as well as the volume fraction of the Si₃N₄ affect composite densification. Inhomogeneous whisker distribution dominated the complete densification of the composites.     

Sol—Gel Processing of SiC-Whisker-Reinforced Silica-Based Ceramic Composites

SiC whiskers were added to reinforce a gel-derived SiO₂–Al₂O₃–Cr₂O₃ matrix. Alumina and chromia were added to induce reaction sintering of the composites. A maximum of ∼90% of theoretical density was achieved after firing in argon for 2 h at 1400°C. The optimum amounts of alumina, chromia, and SiC were 26.5, 1.6, and 4.1 vol%, respectively. It was shown that the chromium acetate hydroxide, used as a precursor for chromia, acted as a gelling agent and as a sintering additive. The effect of producing gaseous products such as SiO, CO and/or CrO₃ became significant above 1400°C where mullite formation also occurred. However, the measured mechanical properties were remarkable, considering the experimental conditions applied.     

Effects of Temperature and Whisker Volume Fraction on Average Residual Thermal Strains in a SiC/Al2O3 Composite

Residual thermal strains in a SiC-whisker-reinforced/Al₂O₃-matrix composite were measured as functions of temperature and volume fraction of whiskers by means of a neutron diffraction technique. The residual strains in both phases decrease with increasing temperature. At room temperature, the residual strains in the whiskers decrease with increasing whisker volume fraction, but the tensile residual strains in the matrix increase. The results agree well with those predicted by an analytical method.     

Micromechanical Stresses in SiC-Reinforced Al2O3 Composites

Applying an Eshelby approach, the internal micromechanical stresses within an SiC-inclusion-reinforced (platelet to whisker geometries) polycrystalline alumina matrix composite were calculated. The results are compared to the experimental residual stress measurements of a SiC-whisker-reinforced Al₂O₃ by Predecki, Abuhasan, and Barrett and found to be in excellent agreement. The calculations are then extended to SiC-reinforced composites with polycrystalline mullite, silicon nitride, and cordierite matrices. It is concluded that the internal stresses are significantly influenced by the inclusion geometry as well as the thermoelastic differences between the inclusion and the matrix and also the volume fraction.     

Tribological Behavior of SiC-Whisker/Al2O3 Composites against Carburized 8620 Steel in Lubricated Sliding

Mineral oil lubricated sliding tests of Sic-whisker (SiC_w,)/A1₂0₃ composites and monolithic alumina against carburized 8620 steel were conducted on a cylinder-on-cylinder machine. The wear rate of the composites was one or two orders of magnitude less than that of pure alumina. Hot-pressed 25 wt% SiC_w,/A1₂0₃ composite had a lower wear rate than sintered and HIPed 7.5 wt% SiC/Al₂O₃ composite under the same conditions. The weight loss of the steel mating ring against the 25 wt% SiC_w, composite was a factor of four lower than against the 7.5 wt% SiC_w, composite, but the former was a factor of 50 to 60 less than that against pure alumina. The composites showed lower friction coefficients than alumina during the run-in stage. The friction coefficients decreased with initial wear. The steady-state friction coefficient decreased with increasing load up to 500 N for hot-pressed 25 wt% SiC,/Al₂0₃ composite. Further, SEM observation showed much less microfracture in composites than in alumina. EDAX analysis revealed less Fe transfer from the steel ring to the composites than to pure alumina. Wear by microfracture and by adhesion in composites was suggested to be suppressed by SIC whiskers. This in turn reduced wear of the steel because of the generation of fewer hard particles.     

Pressureless Sintering of SiC-Whisker-Reinforced Al2O3 Composites: I, Effect of Matrix Powder Surface Area

Pressureless sintering of SiC-whisker-reinforced Al₂O₃ composites was investigated. In Part I of the study, the effect of the matrix (Al₂O₃) powder surface area on densification behavior and microstructure development is reported. Compacts prepared with higher surface area Al₂O₃ powder showed enhanced densification at lower whisker concentrations (5 and 15 vol%). Samples with 15 vol% whiskers could be pressureless sintered to ∼97% relative density with zero open porosity and ∼1.6-μm matrix average grain intercept size.     

Pressureless Sintering of SiC-Whisker-Reinforced Al2O3 Composites: II, Effects of Sintering Additives and Green Body Infiltration

Pressureless sintering of SiC-whisker-reinforced Al₂O₃ composites was investigated. In Part II of the study, the effects of Y₂O₃/MgO sintering additives and green body infiltration on densification behavior and microstructure development are reported. Both sintering additives and green body infiltration resulted in enhanced densification. However, the infiltration approach was more effective for samples with high SiC whisker concentrations. Samples with 27 vol% whiskers could be pressureless sintered to ∼93% relative density and ∼3% open porosity. Fracture toughness values and microstructural features (e.g., grain size) for the infiltrated samples remained approximately the same as observed in the uninfiltrated samples.     

Solubility of Si3N4 in Liquid SiO2

The nitrogen solubility in the SiO₂-rich liquid in the metastable binary SiO₂-Si₃N₄ system has been determined by analytical TEM to be 1%–4% of N/(O + N) at 1973–2223 K. Analysis of the near edge structure of the electron energy loss peak indicates that nitrogen is incorporated into the silicate network rather than being present as molecular N₂. A regular solution model with a positive enthalpy of mixing for the liquid was used to match the data for the metastable solubility of N in the presence of crystalline Si₃N₄ and to adjust the computed phase diagram. The solubility of Si₃N₄ in fused SiO₂ is far less than reported in liquid silicates also containing Al, Mg, and/or Y. Apparently, these cations act as modifiers that break anion bridges in the silicate network and, thereby, allow further incorporation of Si₃N₄ without prohibitive amounts of network cross-linking. Finally, indications emerged regarding the diffuse nature of the Si₃N₄-SiO₂ interface that leads to amorphous regions of higher N content.     

Si3N4/SiC-Whisker Composites without Sintering Aids: I, Quantitative Evaluation of Microstructure

A microstructural evaluation of Si₃N₄ with 20 vol% SiC whiskers, fully densified by hot isostatic pressing (HIP) without sintering aids, is presented. The grain size and morphology of the matrix, the whisker aspect ratio after sintering, interfacial bonding, and the structural stability of reinforcement up to 2000°C are discussed. Image analysis provides quantitative information about whisker dispersion and orientation. It is pointed out that a whisker dispersion and orientation. It is pointed out that a whisker composite with a high degree of homogeneity and isotropy can be obtained by optimizing the mixing procedure and using HIP.     

High-Temperature Mechanical Properties of SiC–Mo5(Si,Al)3C Composites

SiC–Mo₅(Si,Al)₃C composites were fabricated by the melt infiltration process, and the infiltration characteristics were studied in detail. Fracture strength and toughness were measured up to 1600°C using a three-point bending test and indentation strength method, respectively. Both fracture strength and toughness significantly increased at 1400°C with respect to the values at room temperature. These increases were mainly attributed to plastic deformation of the infiltrated Mo₅(Si,Al)₃C phases at elevated temperatures, which acted as ductile toughening inclusions. Compressive creep tests were used to study the creep behavior of the composite in the range of 1550°–1650°C and 150–200 MPa. The stress exponent and activation energy were 1.3 and 277 kJ/mol, respectively. Preliminary oxidation tests showed that the composites exhibited good oxidation resistance at 1500°C because of the formation of a dense oxide scale.     

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.     

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.