Co, $Fe_3O_4$ and Co/$Fe_3O_4$ nanoparticles were synthesized by a polyol process in order to develop their new applications and improve chemical, magnetic properties. The synthesis involved a polyol process using Fe, Co acetylacetonate as precursors and 1-2 hexadecanediol as the polyol. The synthesized $Fe_3O_4$ and Co/$Fe_3O_4$ nanocomposite particles were monodispersed and self arrayed ranging in size of 8~10 and 10~25 nm, respectively. The Co nanoparticle has a crystallite size of 10~40 nm. The synthesized nanoparticles were characterized by their structural, morphological, compositional and magnetic properties using TEM-EDS, XRD, and PPMS techniques.