Abstract A hydrothermal method for preparation of size-controlled Pt nanoparticles dispersed highly on multiwalled carbon nanotubes (Pt/MWCNTs) has been studied to optimize the effective parameters (temperature, time, pH and stirring rate) using Taguchi method. The synthesized Pt/MWCNTs nanocomposite samples were characterized through X-ray diffraction (XRD), transmission electron microscopy (TEM) and X-ray fluorescence (XRF) analyses to identify mean Pt nanoparticles size and Pt content. The analysis of the primary experimental data and demonstration of the main effect trend of each parameter showed that a reaction temperature of about 140 °C, a reaction period of 5 h, a slightly basic reaction pH (∼9) and a stirring rate of 500 rpm are the optimum process conditions which give a low mean Pt nanoparticles size (2.8 nm) and a high Pt content (19.4 wt.%) simultaneously. Cyclic voltammetry (CV) analysis showed that under optimum conditions the synthesized sample gives a specific surface area of 99 m 2 g −1. Obtaining the polarization curves for the two fabricated membrane electrode assemblies (MEAs) using the optimized catalyst and a commercial Pt/C catalyst (10 wt.%, Aldrich) with Pt loading of 0.4 mg cm −2 demonstrated that the catalyst prepared under optimum conditions shows a considerably better performance.