The in-situ chemical oxidative polymerization was introduced to prepare the composites of polyaniline/fullerene (PANI/C 60) in this work. The effects of different reaction conditions such as the concentration of C 60 , the concentration of doping acids, the concentration of aniline (ANI), and the reaction temperature were investigated. The composites were characterized by FTIR, scanning electron microscopy, transmission electron microscope, X-ray diffraction, TGA, X-ray photoelectron spectroscopy, and vector network analyzer measurements. The electromagnetic interference (EMI) shielding properties were evaluated over the frequency range of 1.0-4.5 GHz, and it was found that the average total EMI SE was 23.