The cobalt-containing polyacrylonitrile (PAN) films were fabricated using IR-pyrolysis under low vacuum conditions. It was found that Co/PAN films have a porous structure and cobalt nanoparticles with size 0.1-0.2 μm embedded into PAN matrix. Besides, as a result of interaction between PAN matrix and Co ions unsaturation in the polymer backbone is observed caused by the transformation of the C≡N triple bond to a C=N double bond. At the same time formation of Co-N bond is observed.