A study of the different stages of the electroless deposition of copper on carbon nano fibers activated firstly by a chemical treatment of the carbon nano fiber and secondly by a two-step method has been performed from borth a chemical and a morphological point of view. The combination of XPS measurements and scanning electron microscopy imaging has allowed optimizing the 2 different stage conditions. On a first hand, the different oxide concentration and treatment time of the carbon nano fibers and on a second hand the different conditions of the sensibilisation (Sn bath), activation (Pd bath) and coating (Cu bath) have ben studied. The control of the homogeneity and thickness of copper thin films on carbon nano fiber can be obtained and further more sintered in order to obtain fully dense materials.