Abstract: Catalysts prepared by different approaches show different properties and different catalytic performance. The effects of precursor metal, content of precursor metal, preparing method as well as SnO2 content on the catalytic activity and stability of methane combustion were investigated. Sol-gel method involving supercritical fluid drying technique was employed for the preparation of ZrO2-based materials. Activity evaluation of methane combustion was executed. The results indicated that NiO/SnO2-ZrO2 was a kind of proper catalyst in methane combustion, and most of catalysts led to the full conversion of methane at about 700 ℃ without the production of CO. NiO content is the most important preparation parameter for activity and thermal stability of catalyst, but NiO content influenced the activity and thermal stability of catalysts in an opposite way. X-ray diffraction(XRD) revealed Sn might be advantage of the high temperature stability of ZrO2 powder.