Fe2O3 microsphere is used as iron source and template to prepare Li2FeSiO4/C nanocomposite by a sol–gel method. The carbon content, structure, and morphology of the sample are characterized by carbon–sulfur inferred analysis (CSI), X-ray diffraction (XRD), scanning electron microscope (SEM), and transmission electron microscopy (TEM) techniques. The results show that the Li2FeSiO4/C owns pure phase and sphere-like morphology as a result of an agglomeration of nanoparticles with an average particle size of about 50 nm. The Li2FeSiO4/C exhibits stable cycle performance at different rates from 0.1 C to 2 C, and its capacity at 0.1 C rate can reach 160 mAh g−1.