Abstract: Carbon nanotube-supported platinum nanoparticles (Pt-CNTs) were synthesized using glycol as a reducer and H2PtCl6 as an oxidant under microwave radiation. The CNTs was first hydroxylated in refluxing concentrated HNO3. Transmission electron microscopy was used to investigate the influence of the hydroxylation time on the amount of supported platinum on the carbon nanotubes and the effect of the amount of platinum on the morphology of Pt-CNTs. Selected area electron diffraction, X-ray diffraction, and UV-visible spectroscopy were employed to characterize the structure of the Pt-CNTs and the results showed that Pt was of polycrystal nanoparticles. Cyclic voltammetric study indicated that the CNTs surface was covered by a compact layer of Pt when the loadings of platinum to CNTs was as high as 0.1875 mmol·g-1. The result, on one hand, showed that cyclic voltammetry could be used to study the surface structure and properties of CNTs supported platinum nanoparticles, and on the other hand, indicated that it was possible to obtain novel electrode materials with od catalytic activity and stability by optimizing the synthesizing method for CNTs supported platinum nanoparticles.