Li-storage intermetallic compound FeSb2 was prepared by solvothermal method and was studied as a promising anode material for secondary lithium-ion batteries. The as-prepared powder was characterized by X-ray diffraction (XRD) and field emission scanning electron microscopy (FESEM). The electrochemical Li-storage performances of this intermetallic anode were evaluated in a two-electrode cell Li/LiPF6 (EC+DMC)/FeSb2. It was found that the particle size of FeSb2 powder is in nanoscale and this intermetallic anode exhibited enhanced cycling behavior comparing to its microscaled counterpart prepared by levitation-melting/ball-milling route. Li-storage intermetallic compound FeSb2 was prepared by solvothermal method and was studied as a promising anode material for secondary lithium-ion batteries. The as-prepared powder was characterized by X-ray diffraction (XRD) and field emission scanning electron microscopy (FESEM) . The electrochemical Li-storage performances of this intermetallic anode were evaluated in a two-electrode cell Li / LiPF6 (EC + DMC) / FeSb2. It was found that the particle size of FeSb2 powder is in nanoscale and this intermetalliclic anode showed enhanced cycling behavior comparing to its microscaled counterpart prepared by levitation-melting / ball-milling route.