Nanosized nickel oxide was synthesized by a simple liquid-phase process to obtain the hydroxide precursor and then calcined to form the oxide. The precursor and the nickel oxide were characterized by X-ray diffraction (XRD), infrared spectroscopy (IR), thermal analysis (TG) and temperature-programmed reduction (TPR). The results indicated that the particle size of nickel oxide was controlled by the calcined temperature (T C ). Mixed phases of nickel oxide and nickel hydroxide were present as the T C was lower than 300°C. Non-stoichiometric nickel oxide (NiO x , x = 1.2) was formed between 250°C and 400°C and a pure nickel oxide was formed as the T C arrived 500°C. The particle size of nickel oxide changed as the calcined temperature was controlled under 250°C, 300°C, 400°C and 500°C, the order was 5.6 nm, 6.5 nm, 11 nm and 17 nm, respectively.