Reliable and accurate temperature measurement during microwave processing of ceramic bodies is controversial. Although thermocouples are routinely used in conventional thermal furnaces, their presence in microwave furnaces can locally distort the electromagnetic field, conduct heat away from the sample, induce thermal instabilities and microwave breakdown, and lead to serious measurement errors. These thermocouple effects have been studied and found to be more pronounced in low-and medium-loss ceramic materials. To decrease the thermocouple effects during the processing of advanced ceramic materials, an optical, noncontact temperature sensing system has been developed, calibrated, and incorporated into a computer-controlled microwave furnace.

The thermal conductivity of ZnO with different particle sizes (micrometer, submicrometer, and nanometer) was measured using the laser flash technique. As the "green" samples were heated from room temperature to 600°C (and 1000°C) and then cooled down to room temperature, the thermal conductivity was measured in situ. A model for interparticle neck growth was developed based on mass transfer to the neck region of a powder as a result of known temperature. By combining this model with a three-dimensional numerical code, the thermal conductivity of ZnO was calculated. Excellent agreement between the theoretical calculation and experimental data was found.

During microwave sintering of compacted ceramic powders, the electric field distribution within the ceramic body on a macroscale is determined by a combination of the operating frequency, the sample shape, and its permittivity. In contrast, our studies show that on a microscopic scale, the local electric fields are disproportionately intense close to grain boundaries and rough surfaces due to strong focusing. Also, the electric field in the interparticle contact zone exhibits preferred polarization directions despite illumination by a randomly polarized wave. This can lead to a highly nonuniform energy deposition and accelerated mass transfer rates via ponderomotive diffusion and plasma generation.

Temperature gradients that develop in ceramic materials during microwave heating are known to be strongly dependent on the applied microwave frequency. To gain a better understanding of this dependence, identical samples of ZnO powder compacts were microwave heated at three distinct widely separated frequencies of 2.45, 30, and 83 GHz and the core and surface temperatures were simultaneously monitored. At 2.45 GHz, the approximately uniform “volumetric” heating tends to raise the temperature of the sample as a whole, but the interior becomes hotter than the exterior because of heat loss from the surface. At 30 and 83 GHz, this interior to exterior temperature difference was found to be reversed, especially for high heating rates. This reversal resulted from increased energy deposition close to the sample's surface associated with reduced skin depth. A model for solving Maxwell's equations was incorporated into a newly developed two‐dimensional (2‐D) heat transport simulation code. The numerical simulations are in agreement with the experimental results. Simultaneous application of two or more widely separated frequencies is expected to allow electronic tailoring of the temperature profile during sintering.

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The dependence of the permittivity of porous alumina on the microstructure was studied. Three different algebraic mixing laws inaccurately predicted the measured effective permittivity of the three-phase material, which was alumina, air, and water. Finite-difference electrostatic simulations of physically realistic microstructures accurately predicted the experimental results. The electrostatic simulations also provided physical insight into the arrangement of water in the material and its significant effect on the effective permittivity.

This work is devoted to the theoretical understanding of the microstructure and thermal conductivity relationships of compacted ceramic powders in the initial, nondensifying stage of sintering. A model based on surface diffusion of vacancies for the growth of the neck between particles is combined with numerical fully three-dimensional code calculations, which solve for the effective heat conductivity coefficient of lightly sintered particles. The predictions of the model are in agreement with experimental observations. The approach presented can be applied to solve a series of related problems, like dielectric properties, with arbitrary microstructure and multicomponent composite of the powders.

Microwave sintering, an emerging technology in which the energy is applied directly to the material, enabling rapid sintering, shows potential for the synthesis of advanced ceramic materials with superior properties. The process is complex, combining the propagation and absorption of electromagnetic waves in the ceramic material, heat transport within the geometric body, and densification. The densification changes both macroscopic shape and microstructural morphology. A dynamic balance between the rate of electromagnetic energy absorbed within the bulk of the sample and the rate of energy loss from its surface generally results in temperature gradients. These temperature gradients may be especially important during the microwave sintering of bodies with a complex geometry, because neither the diffusion distance nor the electromagnetic penetration depth scale with sample dimensions. The gradients generated in a ZnO green body of a complex geometry were studied theoretically using various microwave-sintering approaches, and it was found that (1) dual-frequency (2.45 and 30 GHz) microwave processing leads to a decrease in the duration of the temperature gradients, and (2) an increase in the heating rate from 5°C/min to 1400°C/min at 2.45 GHz decreases the total required microwave energy by a factor of 55, while at the same time the internal temperature gradients are maintained over a substantially shorter time.