Abstract: The precursor Sn_0.75Ti(OCH₂CH₂OH)_(7-x) was synthesized by electrolysis of titanium and tin in glycol solution. Nano-crystalline SnO₂/TiO₂ powder was prepared by direct hydrolysis from the precursor and then calcined for 2 h at 400℃. The metal alkoxide was characterized by FT-IR and Raman spectra. The mono-dispersed structure and the diameter of nano-SnO₂/TiO₂ were observed by XRD and SEM.The results showed that SnO₂/TiO₂ of 100~200 nm was obtained in organic solution. The highly active nano-SnO₂/TiO₂ electrode was prepared using electro-synthesis and sol-gel method. The cyclic voltammetry was used to study the redox behavior and electro-catalytic activity of the nano-SnO₂/TiO₂ electrode in HCl/m-NO₂C₆H₄OH solution. The current density of the electrode increased obviously and reached to 143 × 10^-3 A/cm². The electrode potential difference of the redox peaks decreased obviously. The COD removal rate of m-nitrophenol reached to 86.1% and the SnO₂/TiO₂ electrode had high electro-catalytic activities.