A gel/LiMo catalyst was prepared as a cathode material via the sol-gel process and applied calcination at different times. The influence of calcination times, properties and the electrochemical performance of the catalyst were investigated by utilizing cyclic voltammetry, potentiodynamic polarization and electrochemical impedance spectroscopy techniques. The surface of the catalysts, which were prepared in different combinations were physically characterized using X-ray diffraction, scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The SEM and TEM images showed that among the different catalysts, the gel@LiMo catalyst has a different crystal structure. The gel/LiMo catalyst shows good electrochemical performances in an organic solution and has a good structural stability. The catalysts also illustrated great electrochemical performances in the oxygen reduction and evolution reactions. Copyright (C) 2015, Hydrogen Energy Publications, LLC. Published by Elsevier Ltd. All rights reserved.