In this research work, synthesis, characterization and photocatalytic activity of CuFeO2/ZnO nanoparticle for degradation of methylene blue (MB) dyewas studied. The CuFeO2/ZnO nanoparticles were successfully synthesized via successive ionic layer adsorption and reaction (SILAR) method. The crystal structure, vibrational frequency and optical properties of the synthesized CuFeO2/ZnO nanoparticles were studied using x-ray diffraction (XRD), Fourier transform infrared (FTIR) and ultraviolet/visible (UV/vis) spectrophotometers, respectively. The structural characterization of CuFeO2/ZnO nanoparticles has been done by analyzing the results obtained from XRD measurements. The results obtained using the XRD indicates that the desired CuFeO2 phase was synthesized with crystalline size (D) of 22.59 nm. The results obtained using the FTIR spectrum shows peak in the range of 1340-1390 cm-1, ~530 cm-1 and ~420 cm-1 which corresponds for Cu-Fe, Fe-O and Zn-O bond stretching, respectively. Similarly, the results obtained using the UV/vis measurement indicates a red shift in the absorption spectra of ZnO from ultraviolet to visible light due to coupling of CuFeO2 nanoparticle.The photocatalytic applicability of the synthesized CuFeO2/ZnO nanoparticle has been evaluated by photocatalytic removal of MB as a function of time. CuFeO2/ZnO nanoparticle seems promising photocatalyst for degradation of MB under light irradiation with 85.6 % degradation in 60 min. The photocatalytic degradation of MB follows pseudo-first order kinetics with rate constant (k) value of 2.910-2 min−1. Furthermore, the trapping experiment was carried out using different scavenger for active species. Among the active species, hole is the most active species which plays a vital role in the degradation of MB.The results obtained in this research work are in broad agreement with previous experimental findings. Keywords:zinc oxide, cupper iron oxide, methylene blue, photocatalysis, SILAR method,trapping experiment