The LiTi2(PO4)(3) has been successfully synthesized by a PEG (polyethylene glycol, mean molecular weight of 2000) based sol-gel route at a relative low temperature. For further improve its electrochemical properties, a ball milling process with acetylene black has been used to form LiTi2(PO4)(3)/C nanocomposite. The samples are characterized by X-ray diffraction, scanning electron microscopy, and transmission electron microscopy. Electrochemical performance of the samples is characterized by the charge-discharge test and cyclic voltammetry. The results show that the ball milling process enables LiTi2(PO4)(3) nanoparticles networked with conductive acetylene black, which offered higher electrochemical performance. The LiTi2(PO4)(3)/C nanocomposite delivers a higher specific capacity, enhanced rate capability, and better cyclability. (C) 2012 Elsevier Ltd. All rights reserved.