The present paper presents a facile and low-cost liquid-solid interaction chemical method to prepare pure Ni and its alloy with Fe nanoparticles by reducing NiCl2.6H2O and FeCl2.4H2O with aluminum as a reducing agent at room temperature. The structural phase, composition, magnetic properties and morphology of the nanoparticles were monitored by x-ray diffraction (XRD), energy dispersive x-ray analysis (EDX), vibrating sample magnetometer (VSM) and scanning electron microscopy (SEM). The as-prepared Ni nanoparticles are well-defined cubic crystalline structure. In NixFe1-x alloy shows the fcc phase for x=75 at.%, mixture of bcc and fcc phase for x = 0.50 at.%. The magnetization of Ni-Fe alloy nanoparticles increases from 74 to 175 emu/g with Fe percentage.