FeCo alloy is a soft magnetic material that possesses the highest saturation magnetization of 2.4 T and crystallizes in bcc structure as in the case of α-Fe. However, the particles synthesized were highly agglomerated. Thus, in this paper, an attempt was made to control the morphology of the particles using different types and concentrations of surfactants such as oleic acid, oleyl amine, polyvinylpyrrolidone (PVP), etc., during the synthesis of the particles. Though all the surfactant experimented partially prevented the agglomeration, products had larger size distribution except for PVP, which provided nearly monodispersed particles. Furthermore, the FeCo particles synthesized in the presence of PVP were either cubic or nearly spherical depending on the concentration of Fe.