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In this research work novel synthesis of Nickel ferrite nanoparticles NiFe2O4 using Microwave Combustion Method (MCM) has been reported. Stable NiFe2O4 nanoparticles were obtained in an assembly of aqueous solution of metal salt as precursor and black pepper extract as reducing and capping agent subjected to microwaves followed by high temperature in autoclave. Mono disperses ferrite nanoparticles were obtained after completely drying the microwaved assembly. Characterization was carried out through Fourier transform infra-red spectroscopy FTIR and scanning electron microscopy SEM. FTIR revealed presence of amide groups and poly phenols e which were considered to be responsible for reduction of metal cation into its zerovalent state which nucleate to form nanoparticles. SEM was conducted to explore surface morphology of synthesized Nickel ferrite nanoparticles, comes out to be homogeneous and uniformly dispersed with average size lying between 32-34nm. These synthesized nickel ferrite nanoparticles NiFe2O4 possess wide range of applications due to their magnetic, electric, optical and other physical and chemical properties. MCM method provided better yield of metal ferrite nanoparticles with no byproducts and was cheap as compared to chemical methods. The catalytic degradation of dye followed first order reaction kinetics and the maximum degradation efficiency obtained after 40 minutes was 99.85 %.