Abstract
The process of spray drying synthesis of the charge compositions based on silicon nitride α-Si3N4 with organic compounds of aluminum and yttrium in the molar ratio of 3:5 (stoichiometry of yttrium-aluminum garnet) as the sintering additive is considered. The sintered compositions 91.5 % wt. Si3N4 + 8.5 % wt. additive (in terms of garnet) were investigated by X-ray diffraction analysis and scanning electron microscopy as well as by the methods of thermal analysis. The charge compositions were annealed in four stages up to a temperature of 1000℃ in order to decompose organics and form the oxide phase of the sintering additive. High-speed (100 °C/min) spark plasma sintering (SPS) technology was used to produce 10 mm ceramic samples in vacuum, under uniaxial pressure of 70 MPa. The microstructure, mechanical properties and phase composition of ceramics were investigated. Influence of preliminary annealing of charge compositions on structure, phase composition and physical-mechanical properties of ceramics were studied. It is established that preliminary multistage annealing of charge compositions influences the SPS kinetics as well as the density and phase composition of the ceramic. It has been established that the kinetics of SPS of the pre-annealed powders has two-stage character of the shrinkage. In this case denser ceramic microstructure is formed than in the case of reaction synthesis of sintering additive (for charge composition without pre annealing) during the SPS, but pre annealing slows down the growth of elongated β-Si3N4 grains and the volume of sintering additive phase increases. It is shown that in the case of sintering ceramics from unannealed charge compositions the material has lower density but higher hardness. Based on the Yang-Kutler model, the activation energy of the SPS process is determined and it is shown that the compaction kinetics of Si3N4 with sintering additive powders is determined by the intensity of viscous flow of the oxide phase on the grain boundaries of ceramics.
Published Version
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