In this study, we propose the hydrothermal synthesis of binary oxide systems composed of titania and zinc oxide in different molar ratios (TiO2:ZnO = 7:3, 5:5 and 3:7). A detailed investigation was made of the effect of the molar ratio of reagents and the temperature of hydrothermal treatment on the physicochemical and electrochemical properties of the resulting materials. SEM microphotographs show that an increase in the content of ZnO results in the appearance of hexagonal particles, characteristic of that oxide. XRD analysis confirmed that an increase in the contribution of ZnO inhibits the formation of the TiO2 crystalline structure. Analysis of porous structure parameters showed that an increase in the ZnO content leads to a decrease in the BET surface area. The TiO2/ZnO composite electrode exhibited enhanced cyclability and improved stable capacity, relatively good reversibility of cell operation and a wide range of potential as an anode for LIBs. Moreover, the coulombic efficiency of the cell remains higher than 90% over 50 cycles, which indicates the successful accommodation of the mechanical strain upon cycling by the TiO2/ZnO nanostructure. Additionally, X-ray photoelectron spectroscopy was performed to confirm the effective intercalation of lithium ions into TiO2/ZnO material. (C) 2018 The Electrochemical Society.