| Summary: | Lithium–sulfur batteries (LSB) show excellent potential as future energy storage devices with high energy density, but their slow redox kinetics and the shuttle effect seriously hinder their commercial application. Herein, a 0D@2D composite was obtained by anchoring polar nano-TiO<sub>2</sub> onto a 2D layered g-C<sub>3</sub>N<sub>4</sub> surface in situ, and a functional separator was prepared using multi-walled carbon nanotubes as a conductive substrate. Due to their long-range conductivity, multi-walled carbon nanotubes make up for the low conductivity of TiO<sub>2</sub>@g-C<sub>3</sub>N<sub>4</sub> to some extent. A lithium–sulfur battery prepared with a modified separator exhibited excellent long-term cycle performance, a good lithium ion diffusion rate, and rapid redox kinetics. The initial specific discharge capacity of the composite was 1316 mAh g<sup>−1</sup> at 1 C, and a high specific discharge capacity of 569.9 mAh g<sup>−1</sup> was maintained after 800 cycles (the capacity decay rate per cycle was only 0.07%). Even at the high current density of 5 C, a specific capacity of 784 mAh g<sup>−1</sup> was achieved. After 60 cycles at 0.5 C, the modified separator retained the discharge capacity of 718 mAh g<sup>−1</sup> under a sulfur load of 2.58 mg cm<sup>−2</sup>. In summary, the construction of a heterojunction significantly improved the overall cycle stability of the battery and the utilization rate of active substances. Therefore, this study provides a simple and effective strategy for further improving the overall performance and commercial application of lithium–sulfur batteries.
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