Sintering of Nanopowders of Amorphous Silicon Nitride Under Ultrahigh Pressure

Nanopowders of amorphous silicon nitride were densified and sintered without additives under ultrahigh pressure (1.0–5.0 GPa) between room temperature and 1600 °C. The powders had a mean diameter of 18 nm and contained ∼5.0 wt% oxygen that came from air-exposure oxidation. Sintering results at different temperatures were characterized in terms of sintering density, hardness, phase structure, and grain size. It was observed that the nanopowders can be pressed to a high density (87%) even at room temperature under the high pressure. Bulk Si₃N₄ amorphous and crystalline ceramics (relative density: 95–98%) were obtained at temperatures slightly below the onset of crystallization (1000–1100 °C) and above 1420 °C, respectively. Rapid grain growth occurred during the crystallization leading to a grain size (>160 nm) almost 1 order of magnitude greater than the starting particulate diameters. With the rise of sintering temperature, a final density was reached between 1350 and 1420 °C, which seemed to be independent of the pressure applied (1.0–5.0 GPa). The densification temperature observed under the high pressure is lower by 580 °C than that by hot isostatic pressing sintering, suggesting a significantly enhanced low-temperature sintering of the nanopowders under a high external pressure.