Herein, the sol‐gel method is conducted to synthesize the spinel‐layered Li2MnTiO4+z (0.5LiMnTiO4•0.5Li2Mn0.5Ti0.5O3) nanoparticles as a cathode material for Li‐ion batteries. The structural and electrochemical properties of the material are investigated by means of X‐ray diffraction, scanning electron microscopy, electrochemical impedance spectroscopy, and charge‐discharge tests. The obtained sample shows a high capacity of 200 mAh g‐1 with a capacity retention of 90 % after 60 cycles at C/5.