This study was perfomed to manufacture formless ZnO powder into SiO₂/ZnO spherical fine powder by Sol-Gel method. Under N₂ atmosphere the reaction was carried out changing the amount of NH₃ as a catalyst, ethanol as a solvents, water, ZnO seed and varying the reaction temperature and solvent. As a result, we found the fact that we could control particle size SiO₂/ZnO composite by altering molar composition of ethanol and that particle size was decreased as molar ratio of ethanol to TEOS was increased. Besides, we could prepare SiO₂/ZnO composite of which particle size is 0.4 ㎛ and degree of dispersion is good when molar ratio of ethanol to TEOS is 1:146.