Nanosized Pt, Pt-Ru and Pt-CeO2 electrocatalysts supported on acid-treated carbon nanotube (CNT) were synthesized by microwave-assisted heating of polyol process using H2Cl6Pt·6H2O, RuCl3, CeCl3 precursors, respectively, and were characterized by XRD and TEM. And then the electrochemical activity of methanol oxidation for catalyst/CNT nanocomposite electrodes was investigated. The microwave assisted polyol process produced the nano-sized crystalline catalysts particles on CNT. The size of Pt supported on CNT was 7~12 nm but it decreased to 3~5 nm in which 10wt% sodium acetate was added as a stabilizer during the polyol process. This fine Pt catalyst particles resulted in a higher current density for Pt/CNT electrode. It was also found that 10 nm size of PtRu alloys were formed by polyol process and the onset potential decreased with Ru addition. Cyclic voltammetry analysis revealed that the Pt75Ru25/CNT electrode had the highest electrochemical activity owing to a higher ratio of the forward to reverse anodic peak current. And the chronoamperemetry test showed that Pt75Ru25 catalyst had a good catalyst stability. The activity of Pt was also found to be improved with the addition of CeO2.