A series of LiMxFe12xPO4 (M 5 Mg,Zr,Ti) phosphates were synthesized via a sol-gel method. Transmission electron microscopy observations show that LiMxFe12xPO4 particles consist of nanosize crystals, ranging from 40 to 150 nm. High-resolution TEM analysis reveals that a layer of amorphous carbon was coated on the surface of the LiMxFe12xPO4 particles, which substantially increases the electronic conductivity of LiMxFe12xPO4 electrodes. The doped LiMxFe12xPO4 powders are phase pure. Near full capacity ~170 mAh/g! was achieved at the C/8 rate at room temperature for LiMxFe12xPO4 electrodes. The doped LiMxFe12xPO4 electrodes demonstrated better electrochemical performance than that of undoped LiFePO4 at high rate.