A novel three-layer anode having the composition Ti/TiHx/Ni-Sb-SnO2 (Ti/TiHx/NATO) was successfully prepared by a spin-coating and pyrolysis process aiming at a long service lifetime and good electrocatalytic properties for ozone formation. The TiHx as an interlayer was produced by electrochemical cathodic reduction of a coated layer of the TiOx on the titanium substrate. Spin coating and thermal decomposition were used to deposit the Sn-Sb-Ni precursor on the surface of the prepared Ti/TiHx electrode. Cyclic and linear scanning voltammetry, Raman spectroscopy, scanning electron microscopy (SEM) and X-ray diffraction (XRD) were used to reveal the electrode performance and morphology. Results show that the onset potential for the oxygen evolution reaction (OER) of Ti/TiHx /NATO is higher than for Ti/NATO. They also indicate that the service lifetime of the Ti/TiHx/NATO is twice as long as the Ti/NATO at a current density of 50 mA.cm(-2) at room temperature. Electrochemical ozone generation and degradation of the methylene blue were investigated to confirm selectivity and activity of the electrodes. After 5 min electrolysis, a current efficiency for ozone generation of 56% was obtained the electrode with TiHx while 38% was obtained on Ti/NATO under same conditions. The results also confirm that the Ti/TiH x /NATO has a higher kinetic rate constant and decolorization efficiency for removal of the methylene blue compare to the Ti/NATO. The rate constant for the pseudo-first ordered reaction of methylene blue degradation showed high values of 350 x 10(-3) min(-1) for Ti/NATO and 440 x 10(-3) min(-1) for Ti/TiHx/NATO.