Fe-Ni coatings are widely used in electronics industries and its main applications are related to its unique magnetic properties [1]. Some of the important applications of Fe-Ni coatings are in electronic industries, storage, recording and memory devise in computers, magnetic heads for tape recorders and pulse transformers. Metallic nanoparticles are beginning to receive more attention because of their relatively higher chemical activity and specificity of interaction. Control of nanoparticle size, shape and dispersity is the key to selective and enhanced activity [2]. Nano scale composite including iron particles represent a new generation of environmental remediation technologies that could provide low-cost, effective solutions to some of the most challenging environmental clean-up problems. Here, first green strategy for synthesis of Fe-Ni hybrid was reported using 5 mmol of FeCl3.6H2O and Nickel sulfate and extracted solution of Calotropis procera. The Fe-Ni bimetallic nanostructure was gained and characterized using XRD, SEM, EDAX, elemental analysis, XRD and TGA.