Rapid Microwave‐Driven Sulfur Sublimation Synthesis of MS ₂ /RuS ₂ (M = Fe, Co, Ni) for Efficient Alkaline Overall Water Splitting

Abstract Facing the complex application environment and overall inefficiency in the complete water‐splitting process, the development of highly efficient and stable catalytic materials is urgently required. This study innovatively proposes and for the first time implements a rapid synthesis technique driven by microwave‐induced sulfur sublimation, successfully preparing MS ₂ /RuS ₂ (M = Co, Fe, Ni) heterostructure interfaces with high structural stability and uniform active site distribution within merely 60 s. By incorporating iron‐group sulfides, the electronic structure of pyrite‐type RuS ₂ is effectively modulated, enabling the developed MS ₂ /RuS ₂ @G catalyst to exhibit superior activity in alkaline environments. Particularly, the cobalt‐based sulfide regulated pyrite‐type RuS ₂ (CoS ₂ /RuS ₂ @G) achieves a mass activity in the hydrogen evolution reaction (HER) that is 15.4 times that of 20 wt.% Pt/C, and in the oxygen evolution reaction (OER), it surpasses commercial IrO ₂ by two orders of magnitude. This research not only provides a new pathway for enhancing the performance and environmental adaptability of water‐splitting catalysts but also presents a simple and universal method to boost catalytic activity through a synergistic modulation strategy.