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Summary A polyhedral microporous carbon derived from metal‐organic frameworks (ZIF‐8) could present good property for sulfur loading and trapping. A melting‐evaporation route was adopted to synthesize two sulfur/microporous carbon (S/MC) composites, of which sulfur content is controllable, and ether‐based or ester‐based electrolytes were used to evaluate the synthesized composites for the lithium sulfur batteries. According to electrochemical results, the S/MC composite with 65.2 wt% S in the ether‐based electrolyte exhibited optimized performance as compared with the composite with 65.2 wt% S in the ester‐based electrolyte, as well as the composite with 58.6 wt% S in the two kinds of electrolytes. For the S/MC composite with 65.2 wt% S in ether‐based electrolyte, the initial discharge capacity could reach up to 1505.9 mAh g−1 and the reversible capacity could be 833.3 mAh g−1 after 40 cycles at 0.1 C. Furthermore, while being respectively evaluated at 0.5, 1.0, and 2.0 C, the discharge capacities could still maintain at 544, 493 and 354 mAh g−1 after 300, 500, and 800 cycles, demonstrating appreciable cyclic reversibility and rate capability.

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