| Summary: | P2/O3 composite sodium layered oxide has emerged as a promising cathode for high-performance Na-ion batteries. However, it has been challenging to regulate accurately the phase ratio of P2/O3 composite due to their high compositional diversity, which brings about some difficulty in manipulating the electrochemical performance of P2/O3 composite. Here, we explore the effect of Ti substitution and the synthesis temperature on the crystal structure and Na storage performance of Na<sub>0.8</sub>Ni<sub>0.4</sub>Mn<sub>0.6</sub>O<sub>2</sub>. The investigation indicates Ti-substitution and altering synthesis temperature can rationally manipulate the phase ratio of P2/O3 composite, thereby purposefully regulating the cycling and rate performance of P2/O3 composite. Typically, O3-rich Na<sub>0.8</sub>Ni<sub>0.4</sub>Mn<sub>0.4</sub>Ti<sub>0.2</sub>O<sub>2</sub>-950 shows excellent cycling stability with a capacity retention of 84% (3C, 700 cycles). By elevating the proportion of P2 phase, Na<sub>0.8</sub>Ni<sub>0.4</sub>Mn<sub>0.4</sub>Ti<sub>0.2</sub>O<sub>2</sub>-850 displays concurrently improved rate capability (65% capacity retention at 5 C) and comparable cycling stability. These findings will help guide the rational design of high-performance P2/O3 composite cathodes for sodium-ion batteries.
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