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Surface reactions constitute the foundation of various energy conversion/storage technologies such as the lithium–sulfur(Li–S)batteries.To expedite surface reactions for high-rate battery applications demands for in-depth understanding of reaction kinetics and rational catalyst design.Herein,we proposed an in-situ extrinsic-metal etching strategy to activate an inert monometal nitride of hexagonal Ni3N through ironincorporated cubic Ni3FeN.In-situ etched Ni3FeN regulates polysulfide-involving surface reactions at high rates.Advanced electron microscopy was employed to unveil the mechanism of in-situ catalyst transformation.The Li–S batteries modified with Ni3FeN exhibited superb rate capability,remarkable cycling stability at a high sulfur loading of 4.8 mg cm-2,and lean-electrolyte operability.This work opens up the exploration of multimetallic alloys and compounds as kinetic regulators for high-rate Li–S batteries and also unearth the understanding of catalytic surface reactions and the role of defect chemistry.