We have prepared a 4.8V voltage cathode, Li(Ni0.5Mn1.5)O4 using the polymer polyvinylpyrrolidone (PVP) as precursor at temperatures ranging from 700 to 750°C for 6h in air. The Rietveld refined X-ray diffraction patterns of Li(Ni0.5Mn1.5)O4 showed a spinel type structure with a lattice parameter value of ∼8.174(2)Å. The Scanning Electron Microscope (SEM) images showed particle size in the range, ∼100–3000nm. The surface area of the prepared powders was characterized by the Brunauer–Emmett–Teller (BET) technique. Cathodic electrochemical properties were evaluated using cyclic voltammetry (CV) and galvanostatic cycling (GC) in the range 3.5–5.0V vs. Li/Li+ at ambient temperature. CV studies showed a minor peak at ∼4.0V due to the Mn3+/4+ redox couple, and main anodic/cathodic peaks at 4.75/4.6V and 4.8/4.7V corresponding to the Ni2+/4+ redox couples. The GC studies were carried out at the current rates (C/4.5) 30mAg−1 and (C/1.2) 120mAg−1, at room temperature. The reversible capacities of all samples prepared at 700–750°C are in the range, 92–130 (±3)mAhg−1 at the end of 15th cycle. Impedance studies were carried out on a selected cell.