Cobalt ferrite nanocrystals were synthesized under size-controlled conditions in aqueous phase and incorporated into a polyimide matrix at various volumetric loads. Synthesized 20. nm cobalt ferrite single crystals, which exhibited a room-temperature coercivity of 2.9. kOe, were dispersed in polyimide precursor using two techniques: homogenizer and ball milling. These suspensions were then cured to develop the polyimide structure in the resulting nanocomposites. Produced films were characterized by Fourier transform infrared spectroscopy, X-ray diffraction and vibrating sample magnetometry, which confirmed the formation of the desired phases. As expected, the saturation magnetization in the nanocomposites varied according to the polyimide/ferrite weight ratio, while coercivity remained at the value corresponding to pure cobalt ferrite nanocrystals. Thermal degradation, thermal stability and dynamic mechanical analyses tests were also carried out to assess the effect of the concentration of the ferrite disperse phase on the thermo-mechanical behavior of the corresponding nanocomposites as well as the used dispersion techniques. © 2010 Elsevier B.V.