Silicon powder in a reaction-sintered silicon nitride crucible was heated a
t 1600 degrees C in a nitrogen atomosphere. Clustered beta-Si3N4 Single cry
stals were obtained in residual silicon metal after cooling, The silicon re
siduals were dissolved by chemical purification using a mixture of aqueous
HF and HNO3, and subsequently treated and with H2SO4, Scanning electron mic
roscopy observation showed that large beta-Si3N4 crystals without Si residu
als could be successfully separated by this process.