Magnetic nanoparticles are considered as an interesting material owing to their potential applications in biotechnology, medical technology and other related fields. Magnetic nanoparticles can be alloys, metals and its oxides such as ion nanoparticles, ion oxide nanoparticles, iron-cobalt alloy nanoparticles. In this research, magnetic nanoparticles of NiCo alloy were prepared by polyol process with using polyvinyl alcohol (PVA) and ethylene glycol as solvent while sodium borohydride was the reducing agent to reduce Ni2+ and Co2+ ions together in solution. Nanoparticles were characterized using transmission electron microscopy (TEM), X-ray diffraction (XRD) while Vibrating Sample Magnetometer (VSM) was used to characterize the magnetic behaviour of the particles.