The multi-walled carbon nanotubes (MWCNTs) have drawn great attention due to their exceptional mechanical, physical, thermal and electrical properties. The MWCNTs as the reinforcements significantly improved the properties of materials. However, the major challenges in composites containing CNTs are the poor wettability and poor interfacial bonding between matrix and CNTs. In this study, the used MWCNTs have a diameter of 8-10 nm and 1.5 mu m in length. MWCNTs are purified in HNO3: H2SO4, sensitized in Sn solution and activated in Pd solution at 90 degrees C, and coated with the Nickel and Cobalt elements using an electroless coating method. The holding time in the bath is 15, 30 and 60 min, and the bath concentration is also changed. The coatings are characterized by Scanning Electron Microscopy (SEM) equipped with electron dispersive spectrum (EDS), elemental mapping, x-ray diffraction (XRD), Raman spectroscopy, Transmission Electron Microscopy (TEM) and Fourier Transform Infrared (FTIR) spectrometer. The results showed that the Ni and Co coating layers are successfully formed on the surface of MWCNTs. The deposition rate is affected by the holding time and the bath concentration. The optimal results are obtained at the holding time of 60 min in the C concentration sample.