Crack-Healing Behavior of Liquid-Phase-Sintered Silicon Carbide Ceramics

Crack-healing behavior of liquid-phase-sintered (LPS) SiC ceramics has been studied as functions of heat-treatment temperature and crack size. Results showed that heat treatment in air could significantly increase the indentation strength. The heat-treatment temperature has a profound influence on the extent of crack healing and the degree of strength recovery. The optimum heat-treatment temperature depends on the softening temperature of an intergranular phase in each material. After heat treatment at the optimum temperature in air, the crack morphology almost entirely disappeared and the indentation strength recovered to the value of the smooth specimens at room temperature for the investigated crack sizes up to ∼200 μm. In addition, a simple heat treatment of SiC ceramics sintered with Al₂O₃–Y₂O₃–CaO at 1100°C for 1 h in air resulted in even further improvement of the strength, to a value of 1054 MPa (∼150% of the value of the unindented strength). Crack closure and rebonding of the crack wake due to oxidation of cracked surfaces were suggested as a dominant healing mechanism operating in LPS-SiC ceramics.     

Effect of Weight Loss on Liquid-Phase-Sintered Silicon Carbide

The evaporation of silicon carbide (SiC) ceramics during sintering has been studied by thermogravimetry in a graphite furnace filled with argon. The SiC powder compacts contained 7.5 wt% eutectic composition of Y₂O₃–Al₂O₃ to promote liquid-phase sintering. A weight loss of 1–11 wt% was observed during sintering, depending on the sintering temperature and sintering time. The weight loss severely influenced the final density and the microstructure of the SiC ceramics. Particularly, the oxide sintering aids, which were homogeneously distributed in the green ceramics, were observed to segregate and form particular patterns that were dependent on the temperature, sintering time, and the total weight loss. Possible heterogeneous reactions evolving volatile species have been discussed in relation to the experimental observations.     

Core/Rim Structure of Liquid-Phase-Sintered Silicon Carbide

Plasma etching in conjunction with scanning and analytical transmission electron microscopy was used to characterize the microstructure and microchemistry of silicon carbide sintered with yttrium-aluminum garnet (YAG). The SiC grains comprise a core/rim structure with small amounts of excess yttrium, aluminum, and oxygen being present in the rim while these elements are missing in the core. The core/rim interface was found to be coherent, and both the core and the rim are composed of the same polytype, predominantly the 6H structure. These results suggest that Ostwald ripening by solution and reprecipitation controls the sintering mechanism in this system.     

Dynamic Evolution of Grain-Boundary Films in Liquid-Phase-Sintered Ultrafine Silicon Carbide Material

Spatially resolved electron energy-loss spectroscopy (EELS) analysis revealed a dynamic evolution of grain-boundary (GB) films in a liquid phase (Al₂O₃–Y₂O₃–CaO) sintered β-SiC, which had been deformed both in tension and in compression. An effective chemical width was measured from the oxygen segregation to GBs. Significant increase of Al content in GB films was correlated to devitrification of amorphous pockets to form YAG during both deformations. This brought Y into and expelled Al from the pockets. The extra Al was pushed into GBs to form alumina-based films. Al-Y interdiffusion between GB films and pockets is related to deformation time, indicating a constant and limited interdiffusion rate. This evolution of GB films demonstrated that the dynamic process equilibrated these intergranular regions and phases. GB sliding and interdiffusion among intergranular regions were common mechanisms for both deformation modes. Fracture was mainly caused by YAG formation.     

Quantitative Phase-Composition Analysis of Liquid-Phase-Sintered Silicon Carbide Using the Rietveld Method

Accurate quantitative X-ray diffraction analysis of SiC-based ceramics is difficult because of the significant overlap of the Bragg reflections from the different SiC polytypes. In this regard, the Rietveld method is a powerful tool for the accurate and precise analysis of the phase/polytype compositions in these materials. In this study, we have used two different types of Rietveld codes for the quantitative phase/polytype analysis of a liquid-phase-sintered SiC specimen: FULLPROF, which is based on the classical Rietveld approach, and BGMN, which is based on the new fundamental parameter approach. In both cases, the effect of texture corrections on the precision of the analysis also was studied. The accuracy of the analysis, in terms of the weight percentage of SiC (all polytypes) and yttrium aluminum garnet liquid phase, as determined from the starting powder composition, is within the standard deviation of the analysis in both cases (FULLPROF and BGMN), with and without the texture corrections. In addition, in the case of the classical code (FULLPROF), inclusion of the texture corrections has been shown to improve the precision. In contrast, the precision of the analysis using the BGMN code without the texture corrections is better. However, inclusion of the texture corrections is expected to improve the accuracy of the analysis.     

Creep and Microstructural Evolution at High Temperature of Liquid-Phase-Sintered Silicon Carbide

The compressive creep characteristics at 1625°C of liquid-phase-sintered silicon carbide ceramics containing 5 and 15 wt% of crystalline Y₃Al₅O₁₂ (YAG) as the secondary phase were studied. In the two cases, strains between 10% and 15% were reached without failure. The creep behavior was characterized by a stress exponent n ≈2, and the proportion of secondary phase was related to the creep resistance of the materials. The microstructural evolution during creep consisted firstly in the re-distribution of the secondary phase, probably as a consequence of its viscous flow at the creep conditions, and secondly an extensive nucleation and growth of cavities, which was more important for the highest YAG content. The latter reflects the carbothermal reduction that the secondary phase undergoes during creep.     

Microstructural Changes in Liquid-Phase-Sintered Silicon Carbide during Creep in an Oxidizing Environment

The knowledge of the microstructural evolution during exposure to high temperatures is important to understanding the mechanisms responsible for the creep resistance of silicon carbide (SiC) ceramics. This includes not only the phase transformation of the SiC grains, but also the phase transformations of the oxynitride grain-boundary phases. For this study, a series of SiC specimens were prepared with varying molar ratios of AlN-Y₂O₃ additives. Increased creep resistance was observed in specimens with an additive system containing a 2:3 molar ratio or 60 mol% Y₂O₃. A continuous oxide layer of Y₂Si₂O₇ formed at the surface during elevated temperature testing in air. No blistering or cracking was observed in this oxide coating. Further increase of the creep resistance was achieved by a post-sintering nitrogen anneal.     

Phase Transformation and Texture in Hot-Forged or Annealed Liquid-Phase-Sintered Silicon Carbide Ceramics

Starting from three powder mixtures of 80 vol% SiC (100α, 50α/50β, 100β) and 20 vol% YAG, liquid-phase-sintered silicon carbide ceramics were prepared by hot pressing at 1800°C for 1 h under 25 MPa, and then by hot forging or annealing at 1900°C for 4 h under an applied stress of 25 MPa in argon. The phase transformation and texture development in the as-hot-pressed, hot-forged, and annealed SiC ceramics were investigated via X-ray diffraction (XRD) and the pole figure measurements. The 6H → 4H polytypic transformation was observed in samples consisting of both α- and β-SiC phases when subjected to compressive deformation but absent in the case of annealing, suggesting the deformation-enhanced solubility of aluminum in SiC. Deformation was also found to enhance the 3C → 4H transformation in the sample containing entirely β-phase, which is due to the accelerated solution-precipitation process assisted by grain boundary sliding. The current study showed that the β- →α-phase transformation had little effect on texture development in SiC. Hot forging generally produced the strongest texture, with the calculated maximum of 2.2 times random in samples started with pure α-SiC phase. The mechanism for texture development was explained based on the microstructural observations.     

Effect of Sintering Atmosphere on Grain Shape and Grain Growth in Liquid-Phase-Sintered Silicon Carbide

We investigated the effects of the sintering atmosphere on the interface structure and grain-growth behavior in 10-vol%-YAG-added SiC. When α-SiC was liquid-phase-sintered in an Ar atmosphere, the grain/matrix interface was faceted, and abnormal grain growth occurred, regardless of the presence of α-seed grains. In contrast, when the same sample was sintered in N₂, the grain interface was defaceted (rough), and no abnormal grain growth occurred, even with an addition of α-seed grains. X-ray diffraction analysis of this sample showed the formation of a 3C (β-SiC) phase, together with a 6H (α-SiC) phase. These results suggest that the nitrogen dissolved in the liquid matrix made the grain interface rough and induced normal grain growth by an α→β reverse phase transformation. Apparently, the growth behavior of SiC grains in a liquid matrix depends on the structure of the grain interface: abnormal growth for a faceted interface and normal growth for a rough interface.     

碳化硅材料热导率计算研究进展

从声子散射机制出发,介绍了Si C热导率的温度特性和微观导热机理。综述了Si C单晶热导率的2种主要计算方法。Boltzmann-弛豫时间近似(RTA)适用于各个温度段的热导率计算,而分子动力学方法更适用于高温热导率计算。分子动力学方法相比于Boltzmann-RTA方法的优点在于它可以考虑所有高次项的非谐作用。介绍了3种Si C陶瓷热导率近似计算模型,包括界面热阻模型、Debye-Callaway模型及多相系统热导率模型。下一步研究的主要方向仍然是优化计算模型及减少拟合参数。     

反应烧结碳化硅的显微组织及其导电性的研究

研究了液态硅参与下的反应烧结碳化硅的工艺参数、显微组织对其电阻率的影响.随着烧结气氛压力和成型压力增加,反应烧结碳化硅中游离硅量减少,电阻率增加.其烧结机理以碳的溶解及碳化硅的淀析过程为主.     

Thermal Conductivity/Diffusivity of Silicon Carbide Whisker Reinforced Mullite

The thermal conductivity and diffusivity of silicon carbide whisker reinforced mullite was shown to increase with whisker content. This effect was much greater for vapor-liquid-solid (VLS) whiskers than for rice-hull (RH) whiskers. This suggests that the thermal conductivity for the VLS whiskers was significantly higher than for the RH whiskers. Due to preferred orientation of the whiskers, thermal conductivity and diffusivity of the composite samples exhibited significant anisotropy.     

Thermal Diffusivity/Conductivity of Alumina—Silicon Carbide Composites

Thermal diffusivity and conductivity values for several Al₂O₃-SiC whisker composites were determined. The thermal diffusivity values spanned the range from 373 to 1473 K, and thermal conductivity data wre obtained between 305 and 365 K. The thermal diffusivity decreased with increasing temperature and increased with SiC-whisker content. An estimate of the thermal conductivity of the whiskers was obtained from the direct thermal conductivity measurements, but attempts to derive whisker conductivity values from the thermal diffusivity data were not successful because the laser flash method lacks the required accuracy and precision. Specimens were subjected to two different thermal quench experiments to investigate the effect of thermal history on diffusivity. In the most severe case, multiple 1073- to 373-K quenches, radial cracks were observed in the test specimens; however, there was no change in diffusivity. The lack of sensitivity to thermal cycling appears to be related to the sample size.     

Thermal Conductivity of Porous Silicon Carbide Derived from Wood Precursors

Biomorphic silicon carbide (bioSiC), a novel porous ceramic derived from natural wood precursors, has potential applicability at high temperatures, particularly when rapid temperature changes occur. The thermal conductivity of bioSiC from five different precursors was experimentally determined using flash diffusivity and specific heat measurements at temperatures ranging from room temperature to 1100°C. The results were compared with values obtained from object-oriented finite-element analysis (OOF). OOF was also used to model and understand the heat-flow paths through the complex bioSiC microstructures.     

Microstructure, Phase and Thermoelastic Properties of Laminated Liquid-Phase-Sintered Silicon Carbide–Titanium Carbide Ceramic Composites

Hot-pressed silicon carbide–titanium carbide (SiC—TiC) composites sintered with liquid-phase forming Al₂O₃ and Y₂O₃ mixtures have been studied. Samples were fabricated by successively stacking tape-cast sheets of a single composition, resulting in a laminated body of uniform composition. This approach required the development of a technology easily transferable into the production of functionally graded SiC–TiC materials. The effects of this processing route on the resultant microstructures and phases were explored in detail. Additionally, because of the consequences for graded materials, the effects of TiC proportion on the thermal expansion coefficients, Young's modulus, and Poisson's ratios for several SiC–TiC composites were also determined.     

AC Conductivity of Porous Silicon from Monte Carlo Simulations

The AC conductivity of a percolation model with local energetical disorder for porous Silicon in three dimensions, (), is studied by Monte Carlo simulations. The model includes both diffusion and recombination processes and () is obtained by a Fourier transform of the mean-square displacement of the carriers, where hopping diffusion of a single type of carrier (either an electron or an exciton) and two types of carriers (an electron and a hole) are considered. It is found that at low temperatures, the behavior of () depends sensitively on the type of carrier considered.     

氧化铝和碳化硅填充硅橡胶的导热性能研究

研究氧化铝和碳化硅填充硅橡胶的导热性能。结果表明:采用不同粒径碳化硅填充硅橡胶时,随着碳化硅用量的增大,硅橡胶的热导率逐渐增大;在相同填料用量下,粒径小的碳化硅填充硅橡胶热导率高于粒径大的碳化硅填充胶;氧化铝/碳化硅并用填充硅橡胶的导热性能优于单用氧化铝填充胶;当氧化铝/碳化硅质量比为8:2、填充量为600份时,硅橡胶的导热性能最佳。     

Microstructure and Thermal Conductivity of Silicon Carbide with Yttria and Scandia

A fully dense SiC ceramic with high thermal conductivity was obtained by conventional hot pressing, with 1 vol% Y₂O₃–Sc₂O₃ additives. The ceramic had a bimodal microstructure consisting of large and small equiaxed SiC grains. Observation with high‐resolution transmission electron microscopy (HRTEM) showed two kinds of homophase (SiC/SiC) boundaries, that is crystallized and clean boundaries, and a fully crystallized junction phase. The thermal conductivity of the SiC ceramic was 234 W (m·K)^?1 at room temperature. The high thermal conductivity was attributed to a clean SiC lattice and good contiguity between SiC grains.     

Thermal Diffusivity/Conductivity of Magnesium Oxide/Silicon Carbide Composites

SiC-particle-reinforced MgO composites have been fabricated by hot pressing, and the thermal diffusivities of the composites measured in the temperature range 200–1000°C using a laser flash technique. The thermal conductivity of the composites was calculated by multiplying the diffusivity with density and with heat capacity. The Eshelby inclusion model has been examined, and an equation suitable for particulate composites with porosity has been derived using the multiphase Eshelby model. The model also considers the interfacial thermal condition. Good agreement was obtained between the predictions and the experimental results of the thermal conductivity of the composites, even for various levels of porosity in the composites. Crystal defects, observed in the composites, influenced the thermal conductivity, resulting in a deviation from isothermal interfacial condition. This was reflected in the interfacial thermal parameter,β used in the modeling, and the predicted value of β was in the range of 3–10, depending on the thermal conductivity of SiC used for the calculations.     

Silicon Carbide Platelet/Silicon Carbide Composites

α-silicon carbide platelet/β-silicon carbide composites have been produced in which the individual platelets were coated with an aluminum oxide layer. Hot-pressed composites showed a fracture toughness as high as 7.2 MPa·m^1/2. The experiments indicated that the significant increase in fracture toughness is mainly the result of crack deflection and accompanying platelet pullout. The coating on the platelets also served to prevent the platelets from acting as nucleation sites for the α- to β-phase transformation, so that the advantageous microstructure remains preserved during high-temperature processing.