Mullite Coating on Recrytallized Silicon Carbide and Its Cycling Oxidation Behavior

1IntroductionThere are strong interests in identifying approa-ches to protect silicon carbide ceramics from high tem-perature oxidative environments and prolong their serv-ice lives.One method is to apply a refractory coating.The advantage of coating tech…     

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.     

Failure Mechanisms of a Zirconia-8 wt% Yttria Thermal Barrier Coating

Isothermal and cyclic heat treatments of a plasma-sprayed zirconia-8 wt% yttria thermal barrier coating on a nickel superalloy substrate highlighted coating failure mechanisms. A reaction layer formed at the bond coat/ceramic interface, and failure of the coating initiated in the reaction layer due to opening thermal expansion mismatch stresses associated with a nonplanar interface. Crack propagation occurred in the ceramic in all cases, due to the high fracture energy of the interface. The relatively low fracture energy of the coating, in planes parallel to the interface, is the ultimate factor limiting coating lifetime.     

Coal Slag Protection of Silicon Carbide with Chemically Vapor Deposited Mullite Coatings

The corrosion characteristics of bulk alumina, SiC, mullite, and CVD mullite coatings on SiC in contact with coal slag were investigated. Uncoated SiC corroded in the presence of coal slag, forming mixed FeSi phases and carbon. Bulk Al₂O₃ and slag formed a diffusional phase believed to be the spinel hercynite (Fe,Mg)O·(Al,Fe)₂O₃. After exposure to coal slag, a compositional difference was observed at bulk mullite/coal slag interfaces, yet this diffusional phase did not appreciably degrade the mullite samples and no cracking was observed. CVD mullite coatings offered protection to SiC in a simulated coal gasification atmosphere with corrosion protection dependent on the uniformity of the coating. Microprobe analysis of the CVD mullite coating/slag interface showed the formation of a Fe(Mg)Al.     

Thermal Cycling Damage Mechanisms of C/SiC Composites in Displacement Constraint and Oxidizing Atmosphere

A constraint stress of 62.5 MPa is created on a three-dimensional C/SiC composite specimen whose both ends are fixed when temperature is cycled between 900° and 1200°C. The cyclic stress results in a maximum damage strain of 0.06% within 50 cycles owing to coating and matrix cracking, fiber debonding, sliding, and breaking in the composite. This constrained specimen elongation also leads to a final compressive stress of 14 MPa on the composite through a decrease in the baseline constraint stress. Wet oxygen atmosphere at a high cyclic temperature, concomitant with stresses, can aggravate the damage situation by alternate oxidation between internal and external fibers in composites.     

Optimization of Chemical Vapor Deposition Parameters for Fabrication of Oxidation-Resistant Mullite Coatings on Silicon Nitride

Fabrication of mullite (3Al₂O₃·2SiO₂) coatings by chemical vapor deposition (CVD) using AlCl₃–SiCl₄–H₂–CO₂ gas mixtures was studied. The resultant CVD mullite coating microstructures were sensitive to gas-phase composition and deposition temperature. Chemical thermodynamic calculations performed on the AlCl₃–SiCl₄–H₂–CO₂ system were used to predict an equilibrium CVD phase diagram. Results from the thermodynamic analysis, process optimization, and effects of various process parameters on coating morphology are discussed. Dense, adherent crystalline CVD mullite coatings ∼2 μm thick were successfully grown on Si₃N₄ substrates at 1000°C and 10.7 kPa total pressure. The resultant coatings were 001 textured and contained well-faceted grains ∼0.3–0.5 μm in size.     

Microstructural Studies in Alkoxide-Derived Mullite/Zirconia/Silicon Carbide-Whisker Composites

Mullite composites toughened with ZrO₂ (with or without a MgO or Y₂O₃ stabilizer) and/or SiC whiskers (SiC( w )) were fabricated by hot-pressing powders prepared from Al, Si, Zr, and Mg(Y) alkoxide precursors by a sol–gel process. Micro-structures were studied by using XRD. SEM, and analytical STEM. Pure mullite samples contained prismatic, preferentially oriented mullite grains. However, the addition of ZrO₂, as well as the hot-pressing temperature, affected the morphology and grain size in the composites; a fine, uniform, equiaxed microstructure was obtained. The effect of SiC( W ) was less pronounced than that of ZrO₂. Glassy phases were present in mullite and mullite/SiC( W ) composites, but were rarely observed in Al₂O₃-rich or ZrO₂-containing samples. The formation of zircon due to the reaction between ZrO₂ and SiO₂ and the considerable solid solution of SiO₂ in ZrO₂ prevented the formation of the glassy phase, whereas the reaction between Al₂O₃ and MgO in MgO-containing samples formed a spinel phase and also deprived the ZrO₂ phase of the stabilizer. Intergranular ZrO₂ particles were either monoclinic or tetragonal, depending on size and stabilizer content; small intragranular ZrO₂ inclusions were usually tetragonal in structure.     

Effects of Water Vapor on Oxidation of Silicon Carbide

The rate of oxidation of silicon carbide was studied at different partial pressures of water vapor. The diffusion-rate constant was found to vary with the logarithm of the partial pressure of water vapor according to the theory of thin-film oxidation as proposed by Engell and Hauffe. The products of oxidation were cristobalite and tridymite, depending on the temperature. The diffusing species appeared to be the same in the presence of partial pressures of water vapor and in the presence of partial pressures of oxygen.     

Development of Low–Thermal Expansion Mullite Bodies

A series of ceramic compositions based on variations in the crystal–glass ratio of a mullite body were developed. The thermal expansion of these compositions varies from 3.7 to 5.0×10^–6/°C to 800°C. The materials are particularly useful for applications involving silicon, in that an identical thermal expansion is available. The high–temperature creep data for the lower–expansion compositions are inferior as a result of their higher glass contents. Raw material sources and fabrication procedures for specific compositions are given.     

莫来石/刚玉复相陶瓷热断裂特性研究

通过调整复相陶瓷中颗粒相的组成与级配,利用引入的热膨胀失配机制,控制莫来石/刚玉复相陶瓷显微结构,改善高温复相陶瓷热稳定性,着重研究了莫来石/刚玉复相陶瓷的热断裂特性.研究表明,全部采用莫来石颗粒相时,由于柱状莫来石颗粒极易发生热冲击穿晶断裂,且热膨胀失配导致的微裂纹较长,密度较小,故复相陶瓷热稳定性较差;全部采用刚玉颗粒相时,虽然基质相裂纹扩展至刚玉颗粒表面时穿晶断裂与沿晶的裂纹扩展同时发生,有利于改善复相陶瓷热稳定性,但由于热膨胀失配过度,未经热冲击时已产生宏观裂纹,故热稳定性最差.而采用莫来石/刚玉复合颗粒相,相比例为75/25制备的复相陶瓷试样,热膨胀失配形成的微裂纹较短,密度较大,其热稳定性最优.     

Solid Solutions of Silicon Oxide in Mullite

An explanation is proposed to account for the possibility of formation of solid solutions of silicon oxide in mullite. The difference in the diffusion coefficients of cations in complex oxides leads to the formation of a solid solution of the oxide containing the cation with the lower diffusion coefficient in the complex oxide and a phase containing the cation with the higher diffusion coefficient or rich in this oxide. Using yttrium or scandium additives, which are chemisorbed on the surface of aerosil (SiO₂ source), it is possible to make the rate of diffusion mass transfer of aluminum cations higher than that of silicon cations and thus obtain a solid solution of silicon oxide in mullite.     

涂装生产线热循环系统关键组件的优化设计方法研究

合理设计燃油燃气加热器、挡板、搅拌管、控制系统，解决常见的火焰燃烧不充分、排烟温度高、喷淋液温度达不到工艺要求等问题。优化后的系统液槽内液体升温快，燃烧器可以较长小火燃烧时间，排烟温度低。     

Thermal stability of C/Mullite composites in different environments

In the present study, the mechanical properties and microstructure of C/Mullite composites with a PyC-SiC double-layer interfacial coating after annealing were systematically studied to evaluate the evolution of thermal stability in an inert atmosphere and a vacuum. The C/Mullite composites annealed in the inert atmosphere exhibited better thermal stability than those annealed under the vacuum. The main factor for failure of the composites was carbothermal reduction. The activation temperature of carbothermal reduction in composites in the inert atmosphere was ～100 °C higher than that in the vacuum. Once carbothermal reduction was activated, the microstructure of composites was destroyed, resulting in a significant weight loss and mechanical property degeneration. The degeneration of mechanical properties was unrecoverable.     

Reaction Bonding and Mechanical Properties of Mullite/Silicon Carbide Composites

Based on the RBAO technology, low-shrinkage mullite/SiC/ Al₂O₃/ZrO₂ composites were fabricated. A powder mixture of 40 vol% Al, 30 vol% A1₂O₃ and 30 vol% SiC was attrition milled in acetone with TZP balls which introduced a substantial ZrO₂ wear debris into the mixture. The precursor powder was isopressed at 300–900 MPa and heattreated in air by two different cycles resulting in various phase ratios in the final products. During heating, Al oxidizes to Al₂O₃ completely, while SiC oxidizes to SiO₂ only on its surface. Fast densification (at >1300°C) and mullite formation (at 1400°C) prevent further oxidation of the SiC particles. Because of the volume expansion associated with the oxidation of Al (28%), SiC (108%), and the mullitization (4.2%), sintering shrinkage is effectively compensated. The reaction-bonded composites exhibit low linear shrinkages and high strengths: shrinkages of 7.2%, 4.8%, and 3%, and strengths of 610, 580, and 490 MPa, corresponding to compaction pressure of 300, 600, and 900 MPa, respectively, were achieved in samples containing 49–55 vol% mullite. HIPing improved significantly the mechanical properties: a fracture strength of 490 MPa and a toughness of 4.1 MPa^.m^1/2 increased to 890 MPa and 6 MPa^.m^1/2, respectively.     

Study of Grass Shoot-Shape Silicon Nanowires Grown by Thermal Chemical Vapor Deposition

Silicon - Grass shoot-shape silicon nanowires (SiNWs) with sharp tip have been successfully synthesized on an n-type Si (111) substrates at temperatures of 700 °C and various times...     

Reactive Coating of Zircon on Mullite and Mullite—Alumina Substrates

A stable zirconia coating of 20–30 pm thickness on a mullite substrate with a different alumina/silica ratio was obtained by reactive coating of zircon. It is shown that the Al₂O₃/ SiO₂ ratio of the mullite substrate drastically affects the morphology of the zirconia coating. The results are explained on the basis of the Al₂O₃–SiO₂–ZrO₂ phase equilibria.     

Dependence of Oxidation Modes on Zirconia Content in Silicon Carbide/Zirconia/Mullite Composites

Two basic oxidation modes of silicon carbide/zirconia/mullite (SiC/ZrO₂/mullite) composites were defined based on the plotted curve of the gradient of the silica (SiO₂) layer thickness (formed on individual SiC particles) versus depth. Mode I, where oxygen diffusivity was much slower in the matrix than in the SiO₂ layer, exhibited a relatively large gradient and limited oxidation depth. Mode II, where oxygen diffusivity was much faster in the matrix than in the SiO₂ layer, displayed a relatively small gradient and an extensive oxidation depth. When the volume fraction of ZrO₂ was below a threshold limit, the composites exhibited Mode I behavior; otherwise, Mode II behavior was observed. For composites with a ZrO₂ content above the threshold limit, the formation of zircon (ZrSiO₄), as a result of the reaction between ZrO₂ and the oxidation product (i.e., SiO₂), might change the oxidation behavior from Mode II to Mode I.     

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.