Nano-sized TiO2 powder was prepared by electrochemical dissolution of spongy titanium in an ethanol solution following direct hydrolysis of the electrolyte solution. Characterization of the electrochemical product revealed that Ti(OEt)(4) was formed by anodic dissolution of spongy titanium in ethanol solution. X-ray diffraction and transmission electron microscope were, respectively, used to investigate the structure of TiO2. This study showed that nano-sized TiO2 prepared by this method has a structural and thermal stability with a narrow size distribution of 5-10 nm. The optimum electrochemical operating conditions established were a temperature of 333-343 K, current density of 400 A m(-2) and faradaic efficiency of 86%. Experiments showed that this process might be recommended as a promising technique for synthesis of nano-sized powder.