Nano-Ni3Sn2 intermetallic compound was successfully prepared by solvothermal method for an anode material of lithium-ion batteries. Its microstructure was characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM) and transmission electron microscopy (TEM). Electrochemical performances were evaluated in a lithium-ion model cell Li/LiPF6 (EC+DMC)/Ni3Sn2. The electrochemical lithiation and de-lithiation behavior of nano-Ni3Sn2 was investigated by ex situ XRD. Diffraction peaks of Ni3Sn2 widened and shrank gradually during lithiation. Sharp Ni3Sn2 peaks appeared again after full de-lithiation. It was proved that nano-Ni3Sn2 could be reversibly charged and discharged with lithium though the de-lithiation capacity of nano-Ni3Sn2 was lower than its theoretical capacity.