Fabrication of Transparent Silicon Nitride from Nanosize Particles

Compaction of ultrafine silicon nitride (Si₃N₄) powder at high pressures and various temperatures followed by pressureless sintering was investigated. The powder, consisting of nearly spherical particles (16 nm in diameter) of amorphous stoichiometric Si₃N₄, was pressed in a diamond anvil cell under pressures up to 5 GPa and temperatures ranging from liquid nitrogen to 500°C. Quality of compaction, evaluated by visual transparency and hardness of the produced compacts, depended on the amount of adsorbed gases on the surface of the particles and on the temperature of compaction. Visually transparent compacts were produced by pressing the starting powder without outgassing in liquid nitrogen under 5 GPa. The transparent compacts exhibited a hardness of 1200 kg/mm² after pressing in the diamond anvil cell at 500°C for 3 h at 5 GPa. After subsequent pressureless sintering conducted for 1 h at 5 GPa. After subsequent pressureless sintering conducted for 1 h at 1400°C in a tube furnace under nitrogen, the hardness of these samples increased to over 2000 kg/mm² and the visual transparency was maintained. The results demonstrated that transparency was maintained. The results demonstrated that transparent compacts of nanosize amorphous Si₃N₄ particles could be sintered to high hardness at relatively low temperatures without using sintering aids or applying pressure during sintering.