In the present work, WO 3 and WO 3 -TiO 2 were prepared by the chemical deposition method. Structural variations, surface state and elemental compositions were investigated for preparation of WO 3 -TiO 2 sonocatalyst. X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive X-ray (EDX) and transmission electron microscopy (TEM) were employed for characterization of these new photocatalysts. A rhodamine B (Rh.B) solution under ultrasonic irradiation was used to determine the catalytic activity. Excellent catalytic degradation of an Rh.B solution was observed using the WO 3 -TiO 2 composites under ultrasonic irradiation. Sonocatalytic degradation is a novel technology of treating wastewater. During the ultrasonic treatment of aqueous solutions sonoluminescence, cavitaties and "hot spot" occurred, leading to the dissociation of water molecules. In case of a WO 3 coupled system, a semiconductor coupled with two components has a beneficial role in improving charge separation and enhancing TiO 2 response to ultrasonic radiations. In case of the addition of WO 3 as new matter, the excited electrons from the WO 3 particles are quickly transferred to TiO 2 particle, as the conduction band of WO 3 is 0.74 eV which is −0.5 eV more than that of TiO 2 . This transfer of charge should enhance the oxidation of the adsorbed organic substrate. The result shows that the photocatalytic performance of TiO 2 nanoparticles was improved by loading WO 3.