LiFePO4/C powders were synthesized by ultrasonic spray pyrolysis using carbon powder instead of organic substances as the carbon source. LiFePO4 (LFP) powders containing different types of carbon powders were prepared and used as cathode active materials in lithium ion batteries. The charge-discharge properties of lithium ion batteries with LFP, LFP/AB, and LFP/CNT powders as the cathode material were worse than those of the battery with LFP/sucrose powder as the cathode active material.