TiO2/ZrO2 nanocomposite was obtained by the sonochemical technique. In this method, two separate gels containing zirconium and titanium were prepared and mixed together. The precursor sol of zirconium was prepared from an aqueous solution of ZrCl4. The precursor titanium tetra isopropoxide (TTIP) dissolved in isopropanol. Mixing of Titanium and Zirconium gels was resulted in a yellow TiO2/ZrO2 gel. The precipitate was calcinated in the furnace. The obtained nanopowder characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM) and Fourier transform infra-red spectroscopy (FT-IR).