Low Temperature and Rapid Synthesis of Li‐Rich Li(Li_0.17Mn_0.83)₂O₄ Spinel Cathodes Derived from Metal‐Organic Frameworks for Lithium‐Ion Batteries

Abstract Li‐rich spinel materials (Li_1+xMn_2−xO₄) have shown promise for lithium‐ion batteries. Nevertheless, the preparation of Li_1+xMn_2−xO₄ faces significant challenges due to the difficulty in achieving a balance between well‐crystallized phases and stoichiometric chemistry. Moreover, the synthesis process is highly sensitive to calcination temperature and time, making it susceptible to phase transformations. Therefore, the rational selection of precursors and corresponding calcination procedures is absolutely essential. Herein, we make full use of the nature of metal‐organic frameworks (MOFs) to achieve phase‐controlled synthesis of Li(Li_0.17Mn_0.83)₂O₄ (LMO−F) spinel cathodes in 8 minutes at 500 °C. The composition and structural evolution during the pyrolysis process were systematically investigated to clarify the relationship between precursors and derivatives. Notably, the LMO−F achieved good electrochemical performance with 100.4 mAh g⁻¹ at 50 mA g⁻¹ after 100 cycles.