Li-rich layered oxide Li1.2Co0.13Ni0.13Mn0.54O2 has been successfully re-synthesized using the ascorbic acid leaching solution of spent lithium-ion batteries as the raw materials. A combination of oxalic acid co-precipitation, hydrothermal and calcination processes was applied to synthesize this material. For comparison, a fresh sample with the same composition has been also synthesized from the commercial raw materials using the same method. X-ray diffraction (XRD), scanning electron microscopy (SEM), Xray photoelectron spectroscopy (XPS) and electrochemical measurements are carried out to characterize these samples. XRD results indicate that both samples have the layered alpha-NaFeO2 structures with a space group of R(3) over bar m. No other crystalline phase was detected by XRD. The electrochemical results show that the re-synthesized and fresh-synthesized sample can deliver discharge capacities as high as 258.8 and 264.2 mAh g(-1) at the first cycle, respectively. After 50 cycles, discharge capacities of 225.1 and 228 mAh g(-1) can be obtained with capacity retention of 87.0 and 86.3%, respectively. This study suggests that the leaching solution from spent lithium ion batteries can be recycled to synthesize Li-rich cathode materials with good electrochemical performance. Crown Copyright (C) 2013 Published by Elsevier B.V. All rights reserved.