CoFe₂O₄ (CoFe) nanoparticles were synthesized via a facile surfactant-free sonochemical reaction. For preparation of magnetic polymeric films, CoFe₂O₄ nanoparticles were added to polystyrene (PS). Nanoparticles were characterized using X-ray diffraction (XRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). Magnetic properties of the samples were investigated using an alternating gradient force magnetometer (AGFM). CoFe₂O₄ nanoparticles exhibit a ferromagnetic behaviour with a saturation magnetization of 62 emu/g and a coercivity of 640 Oe at room temperature. By preparing magnetic films the coercivity is increased. The coercivity of PS/CoFe₂O₄ (10%) nanocomposites is higher than that obtained for PS/CoFe₂O₄ (30%).