23:T4f4,Abstract Deep insight into electrochemical reconstruction aids in the decoding of electrocatalytic mechanisms and the development of design principles for advanced catalysts. Despite recent achievements, research concerning cathodic reconstruction is still lacking compared to the anodic variety. This work captures the electroreductive reconstruction dynamics over bimetal Ni–Mo sulfide by various in/ex situ techniques, and whereby cathodic reconstruction is steered with ion regulation to achieve a heterogeneous Ni–Mo–Fe ternary metal hydroxysulfide (NMFSOH) as a robust hydrogen‐evolving catalyst that is competent in industrial‐level water electrolysis. The thermodynamically adaptive heterosynergism in the resultant NMFSOH catalyst can coordinate water dissociation and hydrogenation for the alkaline hydrogen evolution reaction even at high current densities. A flow‐type alkaline water electrolyzer with dual NMFSOH electrodes affords an electricity consumption of 3.99 kW h Nm −3 and an electricity‐to‐hydrogen efficiency of 88.7%, manifesting its competitive cost‐effectiveness toward practical applications. This study showcases ion‐regulatory reconstruction as an effective strategy to construct high‐performance electrocatalysts.24:T52f,Most transition metal-based catalysts for electrocatalytic oxygen evolution reaction (OER) undergo surface reconstruction to generate real active sites favorable for high OER performance. Herein, how to use self-reconstruction as an efficient strategy to develop novel and robust OER catalysts by designing pre-catalysts with flexible components susceptible to OER conditions is proposed. The NiFe-based layered double hydroxides (LDHs) intercalated with resoluble molybdate (MoO₄ ^2- ) anions in interlayers are constructed and then demonstrated to achieve complete electrochemical self-reconstruction (ECSR) into active NiFe-oxyhydroxides (NiFeOOH) beneficial to alkaline OER. Various ex situ and in situ techniques are used to capture structural evolution process including fast dissolution of MoO₄ ^2- and deep reconstruction to NiFeOOH upon simultaneous hydroxyl invasion and electro-oxidation. The obtained NiFeOOH exhibits an excellent OER performance with an overpotential of only 268 mV at 50 mA cm^-1 and robust durability over 45 h, much superior to NiFe-LDH and commercial IrO₂ benchmark. This work suggests that the ECSR engineering in component-flexible precursors is a promising strategy to develop highly active OER catalysts for energy conversion.25:T5a2,

#	Concept	H-Index	Publications	Citations
1	Engineering	3	3	127
2	Chemical Engineering	3	3	127
3	Chemistry	3	3	127
4	Materials Science	3	3	127
5	Batteries	1	1	35

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