2D hierarchical ZnCo 2 O 4 microsheet-coated separators suppress polysulfide shuttling owing to the strong chemical affinity and promote the conversion reaction kinetics of the anchored polysulfide for greatly improved cyclic and rate performances of Li–S batteries. • 2D hierarchical ZnCo 2 O 4 microsheets are synthesized. • 2D ZnCo 2 O 4 -coated separators effectively suppress LiPS shuttling and improve redox kinetics. • 2D ZnCo 2 O 4 -coated separators exhibit a long-term stability. • 2D ZnCo 2 O 4 -coated separators deliver a high areal capacity. Lithium–sulfur (Li–S) batteries are receiving increasing attention as one of the potential next-generation batteries, owing to their high energy densities and low cost. However, practical Li–S batteries with high energy densities are extremely hindered by the sulfur loss, low Coulombic efficiency, and short cycling life originating from the polysulfide (LiPS) shuttle. In this study, two-dimensional (2D) ZnCo 2 O 4 microsheets fabricated by a facile hydrothermal process are employed to modify the separator, for improving the electrochemical performances of Li–S cells. The resulting 2D ZnCo 2 O 4 -coated separator features a coating thickness of approximately 10 μm, high ionic conductivity of 1.8 mS/cm, and low mass loading of 0.2 mg/cm 2 . This 2D ZnCo 2 O 4 -coated separator effectively inhibits LiPS shuttle by a strong chemical interaction with LiPS as well as promotes the redox kinetics by ZnCO 2 O 4 -coated layers, as determined by X-ray photoelectron spectroscopy analysis, self-discharge, time-dependent permeation test, Li symmetric cell test, and Li 2 S nucleation analyses. Consequently, the Li–S batteries based on the 2D ZnCo 2 O 4 -coated separator exhibit a high initial discharge capacity of 1292.2 mAh/g at 0.1 C. Moreover, they exhibit excellent long cycle stability at 1 and 2 C with capacity retention of 84% and 86% even after 800 cycles, corresponding to a capacity fading rate of 0.020% and 0.016% per cycle, respectively. Effectively, these Li–S cells with a high sulfur loading at 5.3 mg/cm 2 and low electrolyte concentration of 9 μL/mg deliver a high discharge capacity of 4.99 mAh/cm 2 after 200 cycles at 0.1 C.