Ni-P-TiO2 nanocomposite coatings with various contents of TiO2 nano-particulates were prepared by electroless technique from Ni-P plating bath containing TiO2 powder. X-ray diffractometer (XRD) and energy dispersive X-ray (EDX) technique have been applied in order to investigate the chemical composition and phase structure of the coatings, respectively. The incorporation of TiO2 nano-particulates was found to be improved by the addition of TiO2 powder to the plating bath. However, it has no significant effect on the wt% of P content in the deposit. Scanning electron microscope (SEM) images showed that the morphology of Ni-P-TiO2 nanocomposite coating is finer and smoother than that of Ni-P coating. The catalytic activity of the prepared electrodes toward electro-oxidation of small organic molecules was studied and their stability with time was investigated. The catalytic activity was found to vary with the amount of the TiO2 embedded into the Ni deposit.(C) 2008 Elsevier B.V. All rights reserved.