Synthesis of ZrO2 nanoparticles in microwave hydrolysis of Zr (IV) salt solutions-ionic conductivity of PVdF-co-HFP-based polymer electrolyte by the inclusion of ZrO2 nanoparticles

摘要

Nanocrystalline ZrO2 particles have been prepared by microwave hydrolysis of Zr(IV) salt solutions at 400 degrees C for 6h. The paper describes the PVdF-co-HFP-ZrO2-based NCPEMs prepared by a simple solvent casting technique. The incorporation of ZrO2 nanoparticles in the PVdF-co-HFP matrix, improved the ionic conductivity due to the availability of a large amount of oxygen vacancies on ZrO2 surface which may act as the active Lewis acidic site that interact with ClO4- ions. On the other hand, a high concentration of ZrO2 [10 wt(%)] leads to depression in ionic conductivity due to the formation of more crystalline phase in the PVdF-co-HFP matrix. DSC, XRD, SEM and DC-polarization studies were carried out. This paper also explores and proposes a structure-conductivity correlation in the PVdF-co-HFP-LiClO4-ZrO2-based NCPEMs system. The proposed correlation is derived from the interpretation of DSC, XRD and AC-impedance measurements. The temperature dependence of the ionic conductivity of NCPEMs follows the Arrhenius behaviour. Finally, the LSV experiment has been carried out to investigate the electrochemical stability in the polymer electrolytes. (c) 2006 Published by Elsevier Ltd.