A nanostructured Sn/TiO 2 /C composite was prepared from SnO, Ti, and carbon powders using a mechanochemical reduction method and evaluated as an anode material in rechargeable Li-ion batteries. The Sn/TiO 2 /C nanocomposite was composed of uniformly dispersed nanocrystalline Sn and rutile TiO 2 in amorphous carbon matrix. In addition, electrochemical Li insertion/extraction in rutile TiO 2 was examined by ex situ XRD and extended X-ray absorption fine structure. The Sn/TiO 2 /C nanocomposite exhibited excellent electrochemical performance, which highlights its potential as a new alternative anode material in Li-ion batteries.