In this paper, a unique processing approach for producing a tailored, externally controlled microstructure in zinc oxide using very high heating rates (to 4900°C/min) in a microwave environment is discussed. Detailed data on the densification, grain growth, and grain size uniformity as a function of heating rate are presented. With increasing heating rate, the grain size decreased while grain size uniformity increased. At extremely high heating rates, high density can be achieved with almost complete suppression of grain growth. Ultrarapid microwave heating of ZnO also enhanced densification rates by up to 4 orders of magnitude compared to slow microwave heating. The results indicate that the densification mechanisms are different for slow and rapid heating rates. Since the mechanical, thermal, dielectric, and optical properties of ceramics depend on microstructure, ultrarapid heating may lead to advanced ceramics with tailored microstructure and enhanced properties.
Microwave energy was used to sinter high thermal conductivity AlN ceramics (160–225 W/mK). The effects of sintering time, temperature, and amount of additive on phase composition, phase distribution, densification behavior, grain growth, and thermal conductivity were studied. The thermal conductivity of AlN was greatly improved by the addition of Y2O3, extended sintering time, and higher sintering temperatures. Thermal conductivity development in Y2O3-doped AlN showed two distinctive time regimes: (i) densification, where full densification, secondary phase formation, concentration and segregation, and rapid purification of AlN grains occur, accompanied by a large increase in thermal conductivity; (ii) postdensification, where grain growth and secondary phase sublimation/evaporation occur, yielding a further increase in thermal conductivity. Our results indicate that microwave sintering is a promising approach for synthesis of high thermal conductivity AlN ceramics.
A multilayer insulation configuration suitable for microwave sintering of ceramics up to 2100°C was designed and tested successfully. The configuration is based on porous, granular BN/ZrO2 fiber composite powder for packed beds and spacer cylinders. This insulation allows stable, controlled microwave sintering and can be modified to microwave process materials with different thermal, dielectric properties with improved properties.
An optical noninvasive, noncontact extensometer was used to measure the shrinkage of zinc oxide powder compacts during sintering. Powder compacts were uniaxially and isostatically pressed from micrometer, submicrometer, and nano powders and sintered in a thermal oven at temperatures up to 1100°C. The nanometer-size sample started to densify at ϳ400°C, about 200°C below the densification threshold of the micrometer-size sample. The results are in good agreement with those obtained using a contact dilatometer.
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