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Development in high-rate electrode materials capable of storing vast amounts of charge in a short duration to decrease charging time and increase power in lithium-ion batteries is an important challenge to address. Here, we introduce a synthesis strategy with a series of composition-controlled NMC cathodes, including LiNi0.2Mn0.6Co0.2O2(NMC262), LiNi0.3Mn0.5Co0.2O2(NMC352), and LiNi0.4Mn0.4Co0.2O2(NMC442). A very high-rate performance was achieved for Mn-rich LiNi0.2Mn0.6Co0.2O2 (NMC262). It has a very high initial discharge capacity of 285 mAh g−1 when charged to 4.7 V at a current of 20 mA g−1 and retains the capacity of 201 mAh g−1 after 100 cycles. It also exhibits an excellent rate capability of 138, and 114 mAh g−1 even at rates of 10 and 15 C (1 C = 240 mA g−1). The high discharge capacities and excellent rate capabilities of Mn-rich LiNi0.2Mn0.6Co0.2O2 cathodes could be ascribed to their structural stability, controlled particle size, high surface area, and suppressed phase transformation from layered to spinel phases, due to low cation mixing and the higher oxidation state of manganese. The cathodic and anodic diffusion coefficient of the NMC262 electrode was determined to be around 4.76 × 10−10 cm2 s−1 and 2.1 × 10−10 cm2 s−1, respectively.

Layered oxides such as the Mn‐rich lithium nickel manganese cobalt oxides are promising next‐generation lithium‐ion battery cathode materials owing to the abundance and environmental benignity of Mn. However, the first‐cycle irreversibility loss and voltage decay remain key drawbacks that need to be addressed urgently. Herein, rational microwave irradiation is used to induce in situ generation of spinel phase in the bulk of a LiMn0.662Ni0.173Co0.165O2 material. The layered‐spinel heterostructured cathode material delivers excellent cycling stability, with a continuous increase in discharge capacity until the 80th cycle at 0.1 C, thereafter showing a capacity decay of 12.9% when further cycled for 70 cycles, while also displaying suppressed voltage decay 4.11 mV cycle−1 throughout these 150 cycles. Electrochemical impedance spectroscopy studies also show improved lithium diffusion kinetics. To establish the underlying science behind the impact of microwave irradiation, several characterization techniques attribute the observed excellent performance to i) lattice expansion, ii) suppressed Li+/Ni2+ cation mixing, iii) fine‐tuned morphology, iv) increased average manganese oxidation state, and v) increased lattice oxygen in the material. This work showcases the potential of microwave‐assisted synthesis methods in designing cathode materials with tuned physico‐chemical properties, and thus improved electrochemistry. Microwave‐assisted synthesis promotes the in situ formation of a spinel phase within the bulk LiMn0.662Ni0.173Co0.165O2 layered material, significantly enhancing the physico‐chemistry of the layered‐spinel heterostructure (including improved morphology, lattice expansion, reduced cation mixing, higher lattice oxygen content). Consequently, the Mn‐rich layered‐spinel cathode exhibits superior electrochemical performance, evidenced by suppressed voltage decay, enhanced capacity retention, improved cycling stability, and greater Li‐ion diffusivity.