Nanosized double substituted LiNi Y Co1−2Y Mn1+Y O4 (Y =0.05, 0.1, 0.25 and 0.45) spinels have been synthesized by a single-step combustion-aided procedure, which use sucrose as fuel. The as prepared samples contained some amorphous organic impurities that were removed after a short heating at 400°C. The samples have been characterized by X-ray diffraction, thermal analysis and transmission electron microscopy. Lattice parameter of the spinels increased with nickel content, and decreased from 400 to 600°C, at which temperature stoichiometric spinels with particle size of ≈20nm were obtained. The electrochemical properties of the 600°C-treated samples in the 5V region have been studied. The sample with composition LiNi0.45Co0.1Mn1.45O4 has shown the best electrochemical performance, with redox potential of 4.6V, capacity of 129.6mAhg−1, cyclability of 99.6% per cycle, and retained the capacity up to 1C rate.