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In this study, b-SiC powder was prepared using a pyrolysed spherical precursor derived from the hydrolysis mixture of phenyltrimethoxysilane and tetraethyl orthosilicate. Before the pyrolysed experiment, an alkoxide precursor was characterised using 29 Si solid nuclear magnetic resonance, Fourier transform infrared spectroscopy and thermogravimetric analysis. The alkoxide precursor was heated at 1800uC for 4 h under an Ar atmosphere. To examine the pyrolysed residue after heat treatment, the sample was collected and analysed with X-ray diffraction. The X-ray diffraction results for the sample show diffraction peaks at ,35, 60 and 73u, which correspond to the b-SiC phase. According to the results of chemical analysis, the SiC content of the powder that was prepared at 1800uC was determined to be 99?4%. The sintering behaviour of the prepared b-SiC powder was examined using B 4 C and C as sintering additives in the temperature range of 1900-2200uC.