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The combination of electrophoretic deposition and electrodeposition was used to prepare multi-walled carbon nanotubes (MWNTs) /metal nanacomposite films. Multi-walled carbon nanotubes with a diameter range of 20 to 30 nm were dispersed in the organic solvent to form stable suspension. The MWNTs film was prepared by EPD using the mixture of acetyleacetone and etanol in a ratio of 1:1 by volume as suspension medium. The nano-sized nickel particles were then deposited on the surface of carbon nanotubes to form carbon nanotubes/nickel nanacomposite films by electrodeposition. SEM and EDS were used to characterize the morphology and composition of the prepared nano-composite films. The results show that nickel nano-particles with high dispersions and high loadings can be coated uniformly on the surface of carbon nanotubes.