In this study, graphene oxide(GO) was prepared from natural graphite by using Hummers method first, and then was reduced to Graphene by sodium borohydride, finally Fe-Ni-P nanoparticles were deposited on Graphene to form Fe-Ni-P/Graphene nanocomposite material by electroless Fe-Ni plating. The effect of graphene and electroless plating parameters upon the microstructures and properties of Fe-Ni-P/Graphene were investigated. The X-ray diffraction reveals that the C axial plan spacing of graphite after oxidation increases from 0.335nm to 0.809nm and graphene is amorphous. The UV-VIS spectrums show the adsorption position is shifted from 230 nm to 266 nm after GO reduction, that proves most of functional groups on GO were removed. The experimental parameters of electroless Fe-Ni plating include insulating oxygen gas, plating temperature, plating time, pH value of plating bath, and ratio of Fe2+/Ni2+. Experimental results show that Fe-Ni-P nanoparticles of size 8 nm are uniform deposited on graphene at pH10, Fe2+/Ni2+=1, 50℃, plating for 3 minutes and using Ar to insulate oxygen. The Fe content of Fe-Ni-P nanoparticles was analyzed by XPS and ICP-MS, that reveals the Fe content and ratio of Fe2+/Ni2+ between 0~7 are in proper direction and the high content of Fe is 29.3at%; to short the plating time to 1 minute the relation of Fe content and ratio of Fe2+/Ni2+is similar, but the surface of Fe-Ni-P contains higher Fe content than Fe-Ni-P nanoparticles. The Fe and Ni content of Fe-Ni-P/Graphene which is deposited at Fe2+/Ni2+ =5, and for 1 minutes is 61.5-74.1wt% by using ICP-MS, and magnetization is 35 emu/g by using VSM.