Kenneth J. D. MacKenzie, Thommy C. Ekström, G. Vaughan White and J. Stephen Hartman
Carbothermal formation of low-z β′-sialon (z=0.5) from halloysite clay has been carried out using two different forms of the necessary additional silicon, namely, finely divided SiO2 (quartz) and elemental Si. XRD and solid-state 29Si and 27Al MAS NMR studies of the early stages of the reaction at 1000–1400 °C show that the SiO2 forms both Si3N4 , via a series of oxynitrides, and SiC. These then react with the mullite produced by thermal decomposition of the clay, to form β′-sialon. The addition of 3 mass% Y2O3 to the reaction mix does not change the reaction sequence, but facilitates the formation of both mullite and β′-sialon, in which it also promotes the formation of Al–N units. Using elemental Si, some SiC is formed, which reacts with the mullite and remaining Si to form O′-sialon, which may then react further with mullite to produce β′-sialon. The addition of Y2O3 forms transient Y2Si2O7 at lower temperatures, but in the later stages facilitates the formation of β′-sialon with respect to O′-sialon.