Samples with general formula LiMn2−xYxO4 (where x = 0.025, 0.05 mol) were successfully synthesized through thermal decomposition of LiMnC2O4 (OAc) precursor, whereas LiMnC2O4 (OAc) precursor was synthesized by the room temperature solid state reaction. The structural, micro-structural and electrochemical features of pure spinel and yttrium-doped samples were investigated. XRD-analysis indicated that all of the prepared samples mainly belong to cubic crystal form with Fd3m space group. Only Y2O3 begins to appear as secondary impurity phase with maximum doping ratio x = 0.05 mol in minor. The electrochemical investigations included cyclic voltammetry, charge–discharge cycling of coin model cells were performed and indicated that substituted spinel with x = 0.025 mol (LiMn1.975Y0.025O4) exhibits best experimental discharge capacity. Visualization studies were also incorporated to prove crystal structure of Y-doped spinel.