Abstract. CeO 2 /ZnO composite nanoparticles are synthesized by using in-situ precipitation method, without any stabilizers, via conventional i.e. non-ultrasound (NUS) and ultrasound-assisted processing technique (US). The structure, morphology, particle size and % weight loss of the synthesized nanoparticles were analyzed by using X-ray powder diffraction (XRD), Thermogravimetric Analysis (TGA), Scanning electron microscopy (SEM) and Transmission electron microscopy (TEM) to establish the formation of core shell type nanomaterials with an average particle size under 15 nm. The effectiveness of the synthesized core shell morphology of CeO 2 /ZnO (catalyst) for the photocatalytic degradation of Rhodamine B (RhB) dye has also been investigated. It has been observed that the catalysts prepared by sonochemical method exhibit higher photocatalytic activity as compared to the catalysts prepared by the conventional method. It was also found that the ultrasound-assisted technique is an energy efficient method as it saves more than 80% of energy along with a substantial reduction in reaction time, as compared to conventional synthesis technique.