In this paper, the preparation methods of NiCo2O4/Ni electrodes for oxygen evolution reaction (OER) are studied. The applied preparation methods in this research are thermal decomposition, electrophoretic deposition and Ni-Co alloy oxidation. The electrocatalytic properties measurement show that electrode prepared by electrophoretic deposition method has relative low overpotential and good electrocatalysis stability for OER in 1M KOH solutions. The thermal decomposition electrode has the highest apparent electrocatalytic properties but with worse stability than electrophoretic deposition electrode. Alloy oxidation method can also prepare NiCo2O4 electrode but the improvement of electrocatalytic properties is not obvious. The research found that electrophoretic deposition method is a promising method to prepare NiCo2O4 electrode. (c) 2005 International Association for Hydrogen Energy. Published by Elsevier Ltd. All rights reserved.