The creation of new materials with enhanced electrochemical and electrocatalytic activities is a very active field of research. Here we report the successful fabrication of a poly(N-methylthionine)/polyaniline (PNMTh/PANI) nanocomposite catalyst with enhanced electrochemical activity formethanol oxidation using an electrodeposition technique. The resultant nanocomposite was characterized by scanning electron microscopy, X-ray photoelectron spectroscopy, Fourier transform infrared spectroscopy, and electrochemical analysis. The PNMTh/PANI nanocomposite shows higher electrochemical catalytic activity for methanol oxidation in neutral and alkaline solutions compared to the neat PNMTh or PANI. The enhanced electrochemical performance of the nanocomposite has been attributed to the synergetic effects between PNMTh and PANI hybrids and the shape effects of their microstructures. (C) 2016 The Electrochemical Society. All rights reserved.