A series of CuO/Ti−Zr−O composites was prepared and applied for CO oxidation. Then, they were further characterized by X-ray diffraction, Brunauer−Emmett−Teller surface area, UV−vis diffuse reflectance measurement, O 2 temperature-programmed desorption, H 2 temperature-programmed reduction, X-ray photoelectron spectroscopy, high-resolution transmission electron microscopy, and in situ diffuse reflectance infrared Fourier transform spectroscopy. Several points were made as follows: (1) This series of 5CuXTZ composites could still maintain the anatase TiO 2 type after the doping of ZrO 2 and CuO. ( 2) CuO species kept a scattered state on Ti−Zr−O support, forming the active Cu + species and oxygen vacancies.(3) This 5CuXTZ catalyst (Ti:Zr = 20:1) displayed the best reductive property because of a higher number of Cu + species and better reductive properties. (4) The CO oxidation over this 5CuXTZ catalyst followed the L−H mechanism.