Composite electrode materials of FeOOH-based particles and carbon powder were prepared with and without heat treatment of composite powder. The composite powder was obtained by hydrolyzing mixed aqueous solutions of FeCl3, Ti(SO4)2 and electron conducting carbon powder as acetylene black (AB) or Ketjen black (KB). FeOOH-based materials formed in the presence of Ti(IV) ions became amorphous and/or low crystalline structure. The composite powder worked as lithium insertion electrode materials in lithium cells using nonaqueous electrolytes including lithium ions. The electrodes exhibited a good cycle performance at large charge–discharge current densities over 5mAcm−2 (4Ag−1 per weight of active material). In addition, it was found that the cycle performance was effective process to be improved by the heat treatment of the composite materials. The composite materials such as amorphous FeOOH, α-Fe2O3, TiO2 and electron conductive powder obtained by the heat treatment are one of the promising candidates as electrode materials for energy storage devices, such as lithium-ion batteries and hybrid electrochemical supercapacitors.