Abstract. Lithium iron phosphate, LiFePO4, was synthesized by hydrothermal process and subsequently coated with carbon by the thermal decomposition of acetylene gas. The products were characterized by XRD, SEM, and TG-DTA. As-synthesized LiFePO4 was submicron sized plate-like particle. After heating at various temperature in nitrogen atmosphere, the particle size and the crystalline sizes were grown with increasing the heating temperature. Above 700°C, the grain growth was remarkably. Carbon coating temperature was set at 500-600°C because of fine particle and good crystallinity. As a carbon raw material, acetylene gas was flowing to the as-synthesized LiFePO4 in nitrogen atmosphere, and the LiFePO4/C composite was obtained. TG curves showed weight loss above 500°C, which was thought to be associated with carbon layer composition.