The sol-gel synthesis of silicon nitride powders has been studied. The precursor gels were prepared from a colloidal dispersion of silicon dioxide and sucrose, with mole ratios of reactants, C/SiO2, ranging from 2 to 4. The carboreduction and nitridation processes were performed at temperatures between 1400-1550 °C under a dynamic nitrogen atmosphere, with a 4 h hold. The optimum C/SiO2 ratio and temperature for preparation of the Si3N4 powders were selected. For the SiO2CN2 system examined, the boundary temperature between Si3N4 and SiC formation was established, in relation to the amount of carbon introduced