In the present work, the effect of the microwave operation parameters on the heating behaviour of ethylene glycol (EG) solution and thereafter on the physicochemical and electrochemical properties of Pt/C catalysts have been investigated. It was Found that the heating efficiency of the pulse mode (PM) of microwave irradiation is higher than that of the continuous mode (CM). The addition of suitable amount of carbon black into EG system can accelerate the heating process of EG solution, while excessive carbon black decreases the heating rate of EG solution. Moreover, the irradiation time and operation mode can significantly affect the performance of Pt/C catalysts. It was found that Pt/C catalyst prepared in the pulse microwave mode of 10s-ON/10s-OFF for 5 pulses, showed the best electrocatalytic activity towards methanol and ethanol electrooxidation with an electrochemical surface area of 111.7 m(2) g(-1) and a peak current density of methanol and ethanol electro-oxidation of 20.9 mA cm(-2) and 26.7 mA cm(-2), respectively. (c) 2011 Elsevier B.V. All rights reserved.