Connecting to various applications of nickel ferrite as a ceramic magnetic nanocomposite in diverse manufacturing and technical categories, it is essential to optimize its optical, magnetic and microstructural characteristics. Hence a facile route was developed to fabricate nickel zinc ferrite (Ni1-xZnxFe2O4) nanocomposites by co-precipitation route. The enviable spinel phase was studied by X-ray diffractometer and the crystallite size was found to vary from 8 to 15 nm. By Transmission Electron Microscopy, the micro structural and speck distribution was found in the range of 5-12.5 nm. Surface characterization was done using the isothermal BET technique which presents a high surface area that is exhibited by synthesized nanoparticles. Using Kubelka-Munk plot, bandgap was found to be decreasing with the increase of Zn concentration.The synthesized Ni(1-x)ZnxFe(2)O(4) was studied for its application in photo-Fenton degradation of organic Methylene blue (MB) dye. The synthesized nanocatalyst can bereused further which makes itself a proficient candidate in industrial effluent degradation.