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LiNi0.5Mn1.5O4 is a potential cathode material for 5 V batteries. This material was prepared by the solid-state redox method using nitrate and acetate based reactants. The precursor material was obtained when the mixture reactants was heated at 500° C for 10 hours and calcined at different temperatures in the range between 650 and 950° C for 12 hours. The structures of the synthesized materials were verified with X- ray diffraction (XRD) measurement and Scanning Electron Microscope (SEM). The charge-discharge technique was determined using Solartron 1470. As calcination temperature increases, the well-ordered crystal growth oriented to [1 1 1] direction shows a clear octahedral morphology, which is the characteristic of the typical cubic spinel. The Li/LiNi0.5Mn1.5O4 prepared from acetate based reactants calcined at 750° C for 12 h delivered the discharge capacity of 140 mAh/g. [ABSTRACT FROM AUTHOR]