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This work aimed to prepare bilayered V2O5 by hydrothermal route from vanadium (III) chloride (VCl3). According to XRD results, bilayered V2O5 showed a large interlayer spacing around 11.3 Å. The electrochemical properties of bilayered V2O5 were carried out by cyclic voltammetry and charge–discharge testing in non–aqueous electrolytes LiPF6 and NaClO4. | Journal of Science and Technology 55 (1B) (2017) 24–29 HYDROTHERMAL SYNTHESIS OF NANO BILAYERED V2O5 AND ELECTROCHEMICAL BEHAVIOR IN NON–AQUEOUS ELECTROLYTES LiPF6 AND NaClO4 Huynh Le Thanh Nguyen1, *, Nguyen Van Hoang2, Nguyen Thi Ngoc Dieu1, Huynh Bang Vy1, Le My Loan Phung1, 2, Tran Van Man2 1 Applied Physical Chemistry Laboratory, Faculty of Chemistry, University of Science–VNUHCM, 227 Nguyen Van Cu, District 5, Ho Chi Minh City, Vietnam 2 Department of Physical Chemistry, Faculty of Chemistry, University of Science–VNUHCM 227 Nguyen Van Cu, Ward 4, District 5, Ho Chi Minh City, Vietnam * Email: hltnguyen@hcmus.edu.vn Received: 30 December 2016; Accepted for publication: 2 March 2017 ABSTRACT This work aimed to prepare bilayered V2O5 by hydrothermal route from vanadium (III) chloride (VCl3). According to XRD results, bilayered V2O5 showed a large interlayer spacing around 11.3 Å. The electrochemical properties of bilayered V2O5 were carried out by cyclic voltammetry and charge–discharge testing in non–aqueous electrolytes LiPF6 and NaClO4. The curves charge–discharge showed that mechanism of insertion/extraction of Li+ ions and Na+ ions were occurred on a solution solid without the phase transition. Moreover, specific capacity for lithium and sodium intercalation of bilayered V2O5 were found out 250 mAh/g and 200 mAh/g, respectively. The kinetic of lithium’s and sodium’s insertion was evaluated by the electrochemical impedance spectroscopy (EIS). The EIS results exhibited a stabilization of charge transfer in both case and a slow kinetic of sodium’s diffusion compared to lithium’s case due to the large ionic radius of sodium. Keywords: electrochemical impedance spectroscopy, kinetics, lithium’s intercalation, sodium’s intercalation, bilayered V2O5. 1. INTRODUCTION In 21th century, rechargeable batteries are main key of modern technology in many applications from portable devices (smartphone, laptop ) to large–scale (hydride electric vehicle–HEV, smart grid