Abstract: A novel type ofthecatalytic nanocompositesfilm, comprising FeP (Fe₂P) nanoparticles embedded in N-doped porous carbon skeleton, was developed via chemical route. First, the aniline monomers gel was synthesized;next, the Fe-doped polyaniline gel was prepared by one-step solution synthesis with aniline and phytic acid as the Cand P-sources, respectively, and with FeCl₃ solution as the dopant; and finally, the Fe-doped polyaniline gel, after freeze-drying, was rapidly pyrolysized at temperature about 800 ~ 900℃ in H²⁺ Ar atmosphere. The microstructures and electro-catalytic behavior of the pyrolysized films were characterized with scanning electron microscopy, transmission electron microscopy and linear sweep voltammetry. The results show that the composites films consisted of the FeP (Fe₂P) nanoparticles embedded in N-doped, highly porous C-skeleton. The nano-composites films displayed the best catalytic activity for both hydrogen evolution and oxygen reduction at 850℃, possibly because of the increased active surfaces of FeP (Fe₂P) nano-particles.