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With high specific surface area, excellent polysulfide conversion activity, and fast electron/ion transfer at the interface, MXene‐derived heterostructures can be employed as catalysts for lithium‐sulfur (Li−S) batteries to accelerate sulfur redox kinetics and suppress shuttle effect. However, the preparation of MXene‐derived heterostructures often requires high‐temperature reactions, which can easily lead to the oxidation of MXene and sacrifice the electrical conductivity. Herein, a catalytic two‐dimensional heterostructure (ZnS/MXene) was successfully synthesized via a mild method. The MXene skeleton retains the original nanosheet structure without oxidation. The in situ‐grown ZnS nanospheres prevent the restacking of MXene nanosheets, which not only increases the active sites, but also guarantees channels for the fast passage of lithium ions. The interfacial built‐in electric field further promotes electron/ion migration, thereby expediting the polysulfide conversion and suppressing the shuttle effect. Consequently, the batteries using ZnS/MXene modified separators exhibit a high initial discharge capacity of 1230 mAh g−1 at 0.1 C and a low decaying rate of 0.082 % per cycle after 500 cycles at 0.5 C. This work offers a reference for the fabrication of MXene‐based heterostructure in Li−S batteries. [ABSTRACT FROM AUTHOR]