Abstract Well crystallized zinc vanadium oxide hydroxide hydrate (Zn 3(OH) 2V 2O 7· nH 2O) nanosheets have been successfully synthesized by a simple hydrothermal method. The products were characterized by X-ray diffraction (XRD), field-emission scanning electron microscopy (FE-SEM), and Raman spectrum. The composition of Zn 3(OH) 2V 2O 7· nH 2O has been studied by thermal analysis (TG, DTA). The results indicate that there are two water molecules in Zn 3(OH) 2V 2O 7· nH 2O molecular formula. Electrochemical properties of Zn 3(OH) 2V 2O 7· nH 2O nanosheets as negative electrode of lithium ion battery were studied by conventional charge/discharge test, which shows steady platform near 1.4 V, suggesting it as an ideal candidate of negative material for lithium ion battery.