A novel TiO2 electrode was obtained by preparing mesoporous TiO2 film on glassy carbon (GC) substrate with the liquid phase deposition process. The electrochemical measurements indicated that the overpotential for the reduction of maleic acid on bare GC was significantly decreased after the electrode surface was covered with electroactive film, demonstrating the electrocatalytic activity of the TiO2 film. However, the TiO2 film showed a strong inhibition to the electron transfer process of [Fe(CN)(6)](3-)/ [Fe(CN)(6)](4-) redox couple. By attaching gold nanoparticles, the sluggish heterogeneous electron transfer kinetics at TiO2 film was effectively improved while the catalytic activity of TiO2 film was retained. (C) 2005 The Electrochemical Society.