Rapid Microwave-Assisted Polyol Reduction for the Preparation of Highly Active PtNi/CNT Electrocatalysts for Methanol Oxidation

PtNi nanoparticle catalysts supported on oxygen functionalized carbon nanotubes were prepared by microwave-assisted polyol reduction using two different modes of irradiation, namely, continuous or pulsed irradiation. The influence of irradiation time or pulse number on catalyst structure and activity in methanol electrooxidation has been studied. Characterization was done with ICP-OES, XRD, TEM, XPS, and XAS to determine composition, morphology, crystal structural and chemical state. The electrocatalytic activity has been evaluated by cyclic voltammetry (CV) and chronoamperometry (CA). PtNi nanoparticles are present in alloy form and are well dispersed on the carbon nanotubes. Pt is in its metallic state, whereas Ni is present in metallic and oxidized form depending on the preparation conditions. The electrocatalytic activity both in terms of surface and mass specific activity is higher than that of the state-of-the-art-catalyst Pt/C (E-TEK). The enhancement of the electrocatalytic activity is discussed with respect to PtNi alloy formation and the resulting modification of the electronic properties of Pt by Ni in the alloy structure. The microwave assisted polyol method with continuous irradiation is more effective in the preparation of PtNi electrocatalysts both in terms of reaction time and activity than the pulsed microwave method.