In this work, two types of hybrid composite materials were elaborated. The first based on polyaniline (PANI) doped Camphor Sulfonic acid (CSA), Carbon-Coated Cobalt (CCo), and FeNi nanoparticles dispersed in polyurethane. A value of 10 4 S/m of conductivity and a 90 dB of shielding effectiveness in multilayer structure were obtained over the 8-18 GHz frequency band. The second type, based on PANI doped para-toluene sulfonic acid (PTSA), dispersed in epoxy resin with FeNi nanoparticles. A thick material with moderate conductivity and high attenuation of electromagnetic waves was obtained. It was found that a PANI-PTSA/FeNi/epoxy resin composite with thicknesses of 9.7 and 6.5 mm had, respectively, reflection loss values of À22 dB at 9.52 GHz, and À20.7 dB at 14.7 GHz. The electromagnetic properties of the elaborated structure hybrid materials can be optimized to increase the electromagnetic reflection-absorption properties. Thus, the obtained structure can be used in shielding and radar absorbing materials applications.