Copper oxide, CuO, are very important components include of high temperature super- conductors, and widely used. The properties of sintered materials were affected by the size and shape of copper oxide with starting materials in the solid-phase reaction. A homogeneous and fine CuO powder was prepared by thermal decomposition of the copper oxalate precursor. Copper oxalate was precipitated by the addition of copper nitrate solution to an oxalic acid solution. The influence of various factors such as temperature, pH, concentration as well as ultrasonic irradiation in the solution were investigated.