Si2N2O powder has been produced by reacting SiO2 and Si3N4 in the presence of a liquid phase obtained by the addition of Al2O3, Y2O3, and MgO. The phase changes occurring during the reaction have been quantified by X-ray diffraction. The reaction has been studied at different temperatures and periods of time. The grain size of the starting materials has a large influence on the conversion to Si2N2O, and, by using a fine-grained SiO2, a substantial conversion to Si2N2O was obtained within 1 h at 1500°C for the Y2O3-containing material.