Abstract

A powder mixture was prepared using α-phase-rich silicon nitride (Si3N4) as the major raw material, with 0.5wt% Yb2O3 as the additive. These powders were fired at 1650–1800°C for 0.5–2h at a nitrogen pressure of 0.1MPa. The effects of firing temperature and holding time on the crystalline phase and microstructure evolution of β-Si3N4 seeds were investigated in detail. The particle size distribution of the β-Si3N4 seeds before and after acid treatment was also evaluated using laser diffraction/scattering. The results show that, even with a low mass fraction of sintering additive, rod-like β-Si3N4 seeds with an average aspect ratio of ~4 could be successfully obtained after firing at 1750°C for 2h. Furthermore, the use of a dilute HF soak for a short period, the resultant powder showed a single peak frequency distribution with a narrow particle size range (D50≈2.5µm). This suggests that the residual crystalline/glassy phase contained in the as-prepared powder is readily attacked by acid rinse, resulting in the subsequent easy separation of the β-Si3N4 seed grains. The present method is therefore a simple and promising procedure for the preparation of highly dispersive rod-like β-Si3N4 seeds for use in the mechanical properties improvement of Si3N4 ceramics.

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