CNTs were decorated with Ni nanoparticles to decrease floatation of CNTs and improve the wettability between CNT and Al melt by electroless plating method. The as-received size of multi-wall CNTs with 99.5% purity was 10~20nm in diameter and 20um in length. Before Ni deposition, the wet ball milling was tried to improve the dispersion of CNTs in the Ni sulfate solution for several hours. After wet ball milling, the Ni electroless platings have been performed for 1hours at electroless deposition temperature. The Ni deposited CNTs have been characterized in respect of dispersion and size changes of CNTs and Ni particles with field emission scanning electron microscopy(FESEM). The deposited Ni nanoparticles onto the CNTs were 50nm in diameter without ball milling, but they increased in size with increasing milling times up to 120nm. Also, the milled CNTs were damaged and changed from its original morphology due to the high ball milling energy. The addition of surfactant improved the distribution and spheroidization of precipitated Ni nanoparticles. From this study, the multi-wall CNTs have been deposited and decorated with spherical Ni nanoparticles by electroless deposition at a proper milling time and surfactant addition.