Abstract: The carbon nanotubes (CNTs) were treated with acids to improve their performance. The plating layers such as Ni, Cu and Ni-Cu formed on the CNTs surface by chemical plating process were investigated. The results of TG, XRD and SEM reveal that the plated metal particle layer can grow in situ and form the nano-sized, uniform and linked stable layer on the surface of CNTs. The crystal structures and distribution states are different among those of Ni, Cu and compound metal plating layer. According to the results from the four-probe and wave-guide method, the conductivity of the plating compound material is 17.3S/cm, and the shielding effectiveness value of the material is about 71 dB, which reaches an excellent level.