 LiCoO2 and LiCuxAlyCo1−x−yO2 (x = 0.05–0.15; y = 0.05–0.15) powders have been synthesized by sol–gel method using malic acid as chelating agent to obtain sub-micron sized particles. The synthesized samples have been subjected to spectral studies viz., differential thermal analysis (TG/DTA), fourier-transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive X-ray analysis (EDAX) and electrochemical characterization. XRD peak reflections of LiCoO2 and LiCuxAlyCo1−x−yO2 exhibit high degree of crystallinity with better phase purity. SEM images of LiCoO2 exhibit an ice cube surface morphology with grains size of 1.5 μm. Doped lithium cobalt oxide shows surface morphology of uniform particle size 2 μm. EDAX peaks confirm the actual composition of Cu, Al, Co and O in LiCoO2 and LiCuxAlyCo1−x−yO2. Charge–discharge studies of undoped LiCoO2 synthesized by sol–gel method deliver maximum an initial discharge capacity of 127 mA h g−1 which corresponds to columbic efficiency of 65 % during the first cycle with capacity fade of 0.13 mA h g−1 cycle−1 over the investigated 10 cycles. Cu and Al doping LiCoO2 exhibit the capacity fade of 0.06, 0.16, 0.14, 0.13 and 01.3 mA h g−1 cycle−1 over the investigated 10 cycles corresponding to columbic efficiency of 74, 75, 73, 73 and 71 with capacity fade of 2, 3, 2, 2, and 2 mA h g−1 cycle−1 at the 10th cycles for Cu: Al doping of 0.1:0.1, 0.13:0.07, 0.07:0.13, 0.15:0.05, and 0.05:0.15 respectively.