Reaction sequences occurring in dense Li-doped sialon ceramics: influence of temperature and holding time

Abstract

Spark Plasma Sintering (SPS) has been used to consolidate a lithium-doped duplex α–β sialon with the overall composition Li0.5Si9.5Al2.5O2.0N14. The kinetics of densification has been studied, and the phase transformation, reactions and grain growth occurring in the dense compacts upon further heat treatment have been investigated. Two sources of Si3N4 powders were used, namely α- and β-Si3N4. Green bodies heated at a rate of 100 °C min−1 yielded fully dense compacts at 1450 °C (α-Si3N4) and 1500 °C (β-Si3N4) without holding, and these compacts consisted mainly of a locally formed liquid and precursor Si3N4 particles. Upon further heating it was observed that α-sialon is formed initially, irrespectively of whether α-Si3N4 or β-Si3N4 powder is used as Si3N4 source; and when α-Si3N4 is used as starting powder, almost monophasic α-sialon compacts are formed before any transformation to β-sialon takes place on further heating. When β-Si3N4 is used as starting powder the formation of β-sialon is kinetically promoted, and compacts containing α-sialon, β-sialon and β-Si3N4 are obtained before the equilibrium phase assemblage is reached, i.e. a lithium-doped duplex α–β sialon ceramic. These observations can be interpreted in terms of the Ostwald step rule. Grain growth does not occur until the equilibrium phase assemblage has been established. The separation of grain growth from densification and phase transformation has implications for preparing Si3N4-based nano-ceramics and provides possibility for further studies of the kinetics of grain growth in Si3N4-based ceramics.