Abstract: Individual CeO2, ZnO and bimetal oxide core shell CeO2/ZnO composite nanoparticles are synthesized without any stabilizers using in-situ precipitation technique. The structure, morphology and particle size of the synthesized nanoparticles were analyzed by using X-ray powder diffraction, scanning electron microscopy and Transmission electron microscopy. Results reveal that the phase structures of CeO2/ZnO are composited by cubic (fluorite) phase of CeO2 and hexagonal (wurtzite) phase of ZnO. Structure characterization of core shell particles by Transmission electron microscopy indicates that the ZnO shell is around 5 nm in thickness and CeO2 core is 9 nm in diameter. The effectiveness of the synthesized CeO2/ZnO used as catalysts for the photocatalytic well as sonocatalytic degradation of Rhodamine B dye has also been investigated. The results showed that Photocatalysis was more efficient than sonocatalysis in degradation of Rhodamine B.