A recycling process involving mechanical, thermal, hydrometallurgical and sol–gel steps has been applied to recover cobalt and lithium from spent lithium-ion batteries and to synthesize LiCoO2 from leach liquor as cathodic active materials. Electrode materials containing lithium and cobalt can be concentrated with a two-step thermal and mechanical treatment. The leaching behavior of lithium and cobalt in nitric acid media is investigated in terms of reaction variables. Hydrogen peroxide in 1M HNO3 solution is found to be an effective reducing agent by enhancing the leaching efficiency. Of the many possible processes to produce LiCoO2, the amorphous citrate precursor process (ACP) has been applied to synthesize powders with a large specific surface area and an exact stoichiometry. After leaching used LiCoO2 with nitric acid, the molar ratio of Li to Co in the leach liquor is adjusted to 1.1 by adding a fresh LiNO3 solution. Then, 1M citric acid solution at a 100% stoichiometry is added to prepare a gelatinous precursor. When the precursor is calcined at 950°C for 24h, purely crystalline LiCoO2 is successfully obtained. The particle size and specific surface-area of the resulting crystalline powders are 20μm and 30cm2 g−1, respectively. The LiCoO2 powder is found to have good characteristics as a cathode active material in terms of charge–discharge capacity and cycling performance.