The inverted Mn is believed to be directly involved in the cation migrations, which would cause voltage hysteresis and irreversible structural evolution after overdischarging. Moreover, the insertion/extraction reaction was experimentally shown to be accompanied by a series of cation redistributions in the spinel framework, which were further supported by density functional theory calculations. Besides the exceptional reversibility of 12% Mg 2+ insertion in Mg 1– xCrMnO 4 ( x ≤ 1), a partially reversible insertion of excess Mg 2+ during overdischarging was also observed. For the first time in multivalent batteries, high-quality operando diffraction data enabled the accurate quantification of cation contents in the host structure. A new custom operando battery device was designed to study the cation migration mechanisms of the MgCrMnO 4 cathode using 0.1 M Mg(TPFA) 2 electrolyte dissolved in triglyme and activated carbon as the anode. A promising high-voltage spinel oxide cathode material MgCrMnO 4 with 18% Mg/Mn inversion was synthesized successfully.
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