Mesoporous zirconia microspheres were prepared by sol-gel method using F127 and sodium dodecyl sulfate (SDS) as templates. The effects of calcination temperature and the content of templates on the structure and properties of mesoporous microspheres were studied. The size of microspheres is uniform, with diameter of about 900μm. It is found that with the increase of the calcination temperature, the specific surface area of the sample decreases, while the average pore diameter has increase trend. After calcined at low temperature, the samples are pure tetragonal zirconia, and there begin to appear monoclinic phase after calcined at 600 ℃. With the same calcination temperature, the specific surface area and pore volume of the sample added more templates are larger. The addition amount of templates has no influence on the phase structure of the sample.