Some copper/zirconia catalysts were prepared by way of deposition-precipitation (DP); for comparison, others were prepared by impregnation (IM) and co-precipitation (CP). Catalytic reactions were carried out in a fixed-bed minireactor with 0.25 ml catalyst. The results have proved that the zirconia aerogel prepared by supercritical fluid drying has higher specific surface area and larger pore volume; the catalyst composition and the catalyst preparation methods and conditions exert influence on the surface structure of catalysts. The DP CuO/ZrO2 catalysts, especially that with CuO/ZrO2 ratio of about 30/70 (wt.%) and calcined at 350 degreesC have finer ultra-fine particles than the others, leading to higher catalytic activity and favoring the methanol synthesis.