Cu and Ce co-doped ZnO powder has been carried out by sol-gel method in order to gain high performance photocatalyst. The structures, morphologies and photocatalytic properties of resultant (Zn 0.97-x Cu 0.03 Ce x O, x = 0.00, 0.02, 0.04, 0.06, 0.08, 0.10) have been investigated by XRD, SEM and the degradation rate of methyl orange. XRD analyses evidenced that the increase of Ce doping concentration will lead to the decrease of the crystal quality of Zn 0.97-x Cu 0.03 Ce x O powders. SEM indicated that the uniformity of particle size and the increase of the dispersion property of the doped sample will be beneficial to the suspension dispersion of the catalyst. At the same time, it can also promote the catalyst absorption of light and reactant molecules. Photocatalytic analysis showed the total degradation rate is close to one time function distribution with time, and the photocatalytic effect is obviously enhanced.