Layered LiMg0.1Co0.9O2 has been synthesized using microwave assisted solution technique. The precursor has been subjected to thermo-gravimetric/differential thermal analysis (TG/DTA) and calcined at 850°C. The precursor and the calcined powders were characterized by X-ray diffraction (XRD) to confirm the formation of single-phase layered material. Fourier transform infrared (FTIR) studies were carried out to understand the nature of the metal–ligand bond and the observations were consistent with the XRD spectrum. Scanning (SEM) and transmission electron microscope (TEM) images have been obtained to understand the surface morphology and the grain orientation of the synthesized material. Coin cells of 2016 type have been assembled using the synthesized layered material as the cathode active material, lithium foil as the counter and reference electrodes and 1M LiPF6 in 1:1 EC/DEC as the electrolyte. Coin cells were assembled and crimp sealed inside an argon filled glove box. The charge/discharge characteristics of the coin cells were evaluated galvanostatically in the potential range 2.7–4.3V. Results indicate that LiMg0.1Co0.9O2 delivers an average discharge capacity of ∼135mAhg−1 over the investigated 20 cycles and is a potential candidate for use as cathode material in lithium rechargeable cells.