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Herein, a simple strategy for developing Ni\u2010Fe\u2010derivative electrocatalysts via phase evolution of NiFe\u2010LDH under controllable annealing temperatures in an argon atmosphere is reported. The optimized catalyst annealed at 340 <jats:sup>o<\/jats:sup>C (denoted NiO\/FeNi<jats:sub>3<\/jats:sub>) exhibits superior HER properties with an ultralow overpotential of 16 mV@10\u00a0mA cm<jats:sup>\u22122<\/jats:sup>. Density functional theory simulation and in situ Raman analyses reveal that the excellent HER properties of the NiO\/FeNi<jats:sub>3<\/jats:sub> can be attributed to the strong electronic interaction at the interface of the metallic FeNi<jats:sub>3<\/jats:sub> and semiconducting NiO, which optimizes the H<jats:sub>2<\/jats:sub>O\u00a0and H\u00a0adsorption energies for efficient HER and OER catalytic processes. This work will provide rational insights into the subsequent development of related HER electrocatalysts and other corresponding compounds via LDH\u2010based precursors.<\/jats:p>","DOI":"10.1002\/smtd.202201472","type":"journal-article","created":{"date-parts":[[2023,2,20]],"date-time":"2023-02-20T03:44:53Z","timestamp":1676864693000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":139,"title":["Phase Evolution on the Hydrogen Adsorption Kinetics of NiFe\u2010Based Heterogeneous Catalysts for Efficient Water Electrolysis"],"prefix":"10.1002","volume":"7","author":[{"given":"Tuzhi","family":"Xiong","sequence":"first","affiliation":[{"name":"College of Materials Science and Engineering Hunan Joint International Laboratory of Advanced Materials and Technology for Clean Energy Hunan University  Changsha 410082 P. R. 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