The results of a study of ultra-rapid (flash) sintering of oxide ceramic materials under microwave heating with high absorbed power per unit volume of material (10–500 W/cm3) are presented. Ceramic samples of various compositions—Al2O3; Y2O3; MgAl2O4; and Yb(LaO)2O3—were sintered using a 24 GHz gyrotron system to a density above 0.98–0.99 of the theoretical value in 0.5–5 min without isothermal hold. An analysis of the experimental data (microwave power; heating and cooling rates) along with microstructure characterization provided an insight into the mechanism of flash sintering. Flash sintering occurs when the processing conditions—including the temperature of the sample; the properties of thermal insulation; and the intensity of microwave radiation—facilitate the development of thermal runaway due to an Arrhenius-type dependency of the material’s effective conductivity on temperature. The proper control over the thermal runaway effect is provided by fast regulation of the microwave power. The elevated concentration of defects and impurities in the boundary regions of the grains leads to localized preferential absorption of microwave radiation and results in grain boundary softening/pre-melting. The rapid densification of the granular medium with a reduced viscosity of the grain boundary phase occurs via rotation and sliding of the grains which accommodate their shape due to fast diffusion mass transport through the (quasi-)liquid phase. The same mechanism based on a thermal runaway under volumetric heating can be relevant for the effect of flash sintering of various oxide ceramics under a dc/ac voltage applied to the sample.

Yb:(LaY)2O3 ceramic samples have been sintered to almost full density in a fast microwave heating process with zero hold time. Rapid densification is observed at heating rates ranging from 50°C to 2400°C/min. The estimated value of the power absorbed in the materials per unit volume is from 10 to 400 W/cm3, which is similar to the processes of flash sintering under an applied dc/ac voltage. The microstructure of the sintered samples exhibits traces of a liquid‐like intergranular phase. The observed flash microwave sintering effect is associated with both preferential microwave absorption and enhanced mass transport within the softened grain boundaries arising due to an elevated concentration of defects and impurities therein. The volumetric nature of microwave heating gives rise to thermal stresses which can act as an additional driving force for sintering. The advantage of the microwave flash sintering process is that no electrodes are needed to supply the power to the articles undergoing sintering.

A 263 GHz continuous-wave (CW) gyrotron was developed at the IAP RAS for future applications as a microwave power source in Dynamic Nuclear Polarization / Nuclear magnetic resonance (DNP/NMR) spectrometers. A new experimental facility with a computerized control was built to test this and subsequent gyrotrons. We obtained the maximum CW power up to 1 kW in the 15 kV/0.4 A operation regime. The power about 10 W, which is sufficient for many spectroscopic applications, was realized in the low current 14 kV/0.02 A regime. The possibility of frequency tuning by variation of the coolant temperature about 4 MHz/1 °C was demonstrated. The spectral width of the gyrotron radiation was about 10(-6).

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