In this study, carboxylic acids, namely concentrated citric acid and ethylene diamine tetra-acetic acid (EDTA) solution, are used as chelators to synthesize Li-rich layered Li 1.2 Ni 0.13 Mn 0.54 Co 0.13 O 2 (LLNMC) by sol-gel method. We investigate the influence of these chelators on the morphology crystal properties and electrochemical performance of LNMC. Based on XRD data, the synthesized materials can be characterized as a combination of two phases, a rhombohedral R-3m phase (LiNi 1/3 Mn 1/3 Co 1/3 O 2) and a monoclinic C2/m phase (Li 2 MnO 3), which, according to the stoichiometry, are xLi 2 MnO 3 •(1-x)LiNi 1/3 Mn 1/3 Co 1/3 O 2 with x = 0.5. The morphology and local structure were studied using electron microscopy (SEM, TEM and HRTEM) and Raman spectroscopy, respectively. A clear evidence for the effect of chelating agent was observed from electrochemical tests carried out by galvanostatic charge-discharge cycling and electrochemical impedance spectroscopy. The sample prepared via EDTA as organic complexing agent exhibits the best electrochemical properties, with higher capacity and rate capability.