Synthesis of electrochemically active carbon fluorides was achieved through the high-energy milling of graphite or carbon black with CoF3 at room temperature. The carbon fluorides were characterized by elemental analysis, X-ray diffraction, IR, and X-ray photoelectron spectroscopy. The results for the carbon fluoride powder prepared from graphite are reported here. This material, with the formula C1.6F, appears to have both semi-ionic and covalent CF bonds and demonstrates many of the characteristics of low-temperature carbon fluorides. The material has a high discharge potential of 3.2 V vs Li/Li+ and a discharge capacity in the range of 450-500 mAh/g to 2.0 V.