The development of CuO/CeO2 nanocomposites as the sensing material of semiconductor gas sensors is reported.CuO/CeO2 nanocomplex oxide is prepared by modified sol-gel method that uses copper nitrate, cerium nitrate and ethylene glycol as precursors. The optimized synthesis parameters and processing condition have been established. The particle size and distribution, phase morphology, specific surface, electronic states of atoms and gas sensing properties have been systematically characterized by Transmission Electron Microscope (TEM), Brunauer Emmett Teller (BET), X-ray diffraction (XRD), X-ray Photoelectron Spectroscopy (XPS) and gas sensitivity measurement. The results show that the sensor sensitivity depends on particle size, Cu/Ce cation ratio and calcination temperature. The effects of calcinations temperature and CuO loading on the gas sensitivity are also examined. The optimum calcination temperature and the CuO content for the highest sensitivity are 600 ℃ and 12%, respectively. The combination of excellent thermal stability.and tunable sensing properties through careful control of the processing parameters and selection of material composition gives rise to novel nanocomposites attractive to the sensitive and selective detection of a variety of toxic and combustible gases.