Sodium iron silicate (NaFe(III)[SiO 3 ] 2 ) nanorods have been synthesized using iron nitrate (Fe(NO 3 ) 3 ) and sodium silicate (Na 2 SiO 3 ) solutions by means of hydrothermal method. The mixture solution is processed in hydrothermal autoclave first at 180–200 °C for two days and then dried at 70 °C to obtain nanotructured NaFe(III)[SiO 3 ] 2 . It was revealed that NaFe(III)[SiO 3 ] 2 nanorod with the average diameter of ~15 nm and length of several hundreds nm was confirmed by X-ray power diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). Cyclic voltammeter (CV) and electrochemical impedance spectra (EIS) investigations show that this kind of NaFe(III)[SiO 3 ] 2 nanostructures have evident and stable electrochemical redox behavior between potential range of −0.1–0.55 V in alkaline solution.