Fuel cells, particularly direct methanol fuel cells (DMFCs), have great potential as mobile power sources. It has been extensively reported that the DMFC performance strongly depends on the electrode catalyst, and many research groups have focused on the preparation of high efficiency cathode catalysts using all types of metal nanoparticle and support. However, most of these methods are either time-consuming with multiple-steps or there is low loading of the nanocatalyst dispersed on the supports. In this study, platinum nanoparticles of uniform diameter (approximately 4.3 nm) were efficiently dispersed on multi-walled carbon nanotubes (MWCNTs) by the temperature-controlled, microwave-assisted polyol method with the addition of sodium dodecyl sulfate (SDS) and [poly(vinyl pyrrolidone)] (PVP). The addition of SDS and PVP in chloroplatinic acid/ethylene glycol (EG) solution can cause the efficient and homogeneous dispersion of the catalyst particles on MWCNTs, enhance the adsorption of platinum particles, and reduce the residue of platinum particles. Moreover, temperature was determined to be the most important factor affecting the reduction of Pt in the process, and large amounts of Pt particles were characterized when the temperature ranged from 140 to 160 C. The results indicate that the optimum temperature ranges from 140 to 160 C, and that the loading amount of Pt/CNTs can reach more than 50 wt % in only 90 s of processing time. The significant improvements in dispersion and loading are due to the ability of SDS, to wrap the PVPstabilized Pt nanoparticles around the surface of the carbon nanotubes. The characterization analyses were conducted by scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffractometry (XRD), X-ray photoelectron spectroscopy (XPS), and thermal gravimetric analysis (TGA).