The current study is concerned with the preparation and characterization of tantalum oxide-loaded Pt (TaOx/Pt) electrodes for hydrogen spillover application. XPS, SEM, EDX and XRD techniques are used to characterize the TaOx/Pt surfaces. TaOx/Pt electrodes were prepared by galvanostatic electrodeposition of Ta on Pt from LiF-NaF (60:40 mol%) molten salts containing K2TaF7 (20 wt%) at 800 degrees C and then by annealing in air at various temperatures (200, 400 and 600 degrees C). The thus-fabricated TaOx/Pt electrodes were compared with the non-annealed Ta/Pt and the unmodified Pt electrodes for the hydrogen adsorption/desorption (H-ads/H-des) reaction. The oxidation of Ta to the stoichiometric oxide (Ta2O5) increases with increasing the annealing temperature as revealed from XPS and X-ray diffraction (XRD) measurements. The higher the annealing temperature the larger is the enhancement in the H-ads/H-des reaction at TaOx/Pt electrode. The extraordinary increase in the hydrogen adsorption/desorption at the electrode annealed at 600 degrees C is explained on the basis of a hydrogen spillover-reverse spillover mechanism. The hydrogen adsorption at the TaOx/Pt electrode is a diffusion-controlled process. (C) 2010 Elsevier Ltd. All rights reserved.