Free-standing multiwalled carbon nano tube papers (buckypapers) were prepared by vacuum filtration from functionalized multi walled carbon nano tubes (MWCNTs) with controlling porosity. Double phase matrix Sn/SnO2/MWCNT nanocomposites were obtained in two steps, including thermal evaporation of metallic tin (Sn) on the MWCNT papers and RF plasma oxidation. The ratio between metallic tin (Sn) and tin oxide (SnO2) was controlled with plasma oxidation time. It was determined that the evaporated pure tin nano crystals were mechanically penetrated into pores of buckypapers to form functionally gradient nanocomposites. Sn/SnO2 coated on MWCNT buckypapers were used as working electrodes in assembled as coin-type (CR2016) test cells. X-ray diffraction (XRD) and scanning electron microscopy (SEM) were used to determine the structure and morphology of the obtained nanocomposites. In addition, the discharge/charge test, cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS) were carried out to characterize the electrochemical properties of these composites as anode materials for Li-ion batteries. (C) 2013 Elsevier B.V. All rights reserved.