The development of composite materials containing small metal or metal oxides particles has attracted a great deal of attention for their interesting chemical, physical and magnetic properties, providing their use for several technological applications. However, it is necessary that a complete evaluation of the morphological features of these composite be performed and correlated to the above mentioned properties. Therefore, the aim of this work was to use VP-SEM and AFM to investigate the morphology and the phase difference of composite materials based on styrene (STY) and divinylbenzene (DVB), containing iron particles. MFM analysis was also carried out to verify the magnetic properties of surface iron particles.