In the present study, the influence of the temperature–time mode of crystallization (TTC) on the morphology and thermal properties of PP/Fe3O4 nanocomposite materials was investigated. The morphology of the nanocomposites prepared in different TTC mode was studied by atomic force microscope. AFM study shows that the root mean square roughness of samples is 90–95, 50, 21 nm for PP/Fe3O4@20, PP/Fe3O4@200 and PP/Fe3O4@20000 respectively. Thermo gravimetric analysis was employed to investigate the thermal stability of PP/Fe3O4 nanocomposites obtained applying different TTC modes.