Abstract: Sol-gel method involving supercritical fluid drying technique was employed for the preparation of ZrO2-based materials, and NiO/CuO-ZrO2 catalysts were prepared. Reaction activity evaluation was carried out in a micro-reactor with gas chromatograph with the rise of temperature up to 1 000 ℃, and the results indicated that NiO/CuO-ZrO2 was a kind of proper catalyst in methane combustion, and most of the catalysts led to the full conversion of methane at about 700 ℃ without the production of CO. The effect of calcination temperature, CuO and NiO contents were investigated for the catalytic activity and stability of methane combustion at high temperature(1 000 ℃). Also the BET surface area, pore size distribution and X-ray Diffraction (XRD) pattern were measured. The results show that proper calcination temperature is 500 ℃, and when both NiO and CuO contents are 5 mol%, the catalyst shows high activity at relative low temperature, and when both NiO and CuO contents are 15 mol%, the catalyst shows high stability at high temperature.