Many fundamental studies have been carried out regarding waste water and hazardous gas treatment technology using the photolysis effect of TiO2. However, photolysis of both organic and organic-inorganic binders immobilizing TiO2 makes permanent use impossible. In this study we manufactured a catalytic electrode by nickel-TiO2 composite plating in order to immobilize TiO2. The surface properties according to the current density changes of cathode and concentration changes of TiO2 powder in nickel plating bath has been analysed with EDX, XRF, SEM, Raman spectrometer etc. The characterization of the catalytic electrode in decomposition of organic compound has been obtained by using UV-Visible spectrophotometer through analysing concentration changes of methyl orange solution containing the catalytic electrode vs. time with projecting UV-light in the solution. The study shows that a catalytic electrode of nickel-TiO2 composite plating with high-efficiency in decompostion of organic compound has been formed under high concentration of TiO2 powder and low current density of cathode.