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In this work, an efficient optimization strategy is proposed by co\u2010modulating the dual anions (C and S) in Ni<jats:sub>3<\/jats:sub>C\/Ni<jats:sub>3<\/jats:sub>S<jats:sub>2<\/jats:sub>, the heterostructured electrocatalyst, which is prepared via a simple hot\u2010injection method. The presence of Ni<jats:sub>3<\/jats:sub>C\/Ni<jats:sub>3<\/jats:sub>S<jats:sub>2<\/jats:sub> heterojunctions accelerates the charge carrier transfer and promotes the generation of active sites, enabling the heterostructured electrocatalyst to achieve current densities of 10\/100\u00a0mA cm<jats:sup>\u22122<\/jats:sup> at 1.37\u00a0V\/1.53\u00a0V. The Faradaic efficiencies for formate production coupled with hydrogen evolution approach 100%, accompanied with a stability record of 350\u00a0h. Additionally, operando electrochemical impedance spectroscopy (EIS), in situ Raman spectroscopy, and density functional theory (DFT) calculations further demonstrate that the creation of Ni<jats:sub>3<\/jats:sub>C\/Ni<jats:sub>3<\/jats:sub>S<jats:sub>2<\/jats:sub> heterointerfaces originating from dual anions\u2019 (C and S) differentiation is effective in adjusting the <jats:italic>d<\/jats:italic>\u2010band center of active Ni atoms, promoting the generation of active sites, as well as optimizing the adsorption and desorption of reaction intermediates. This dual anions co\u2010modulation strategy to stable heterostructure provides a general route for constructing high\u2010performance transition metal\u2010based electrocatalysts.<\/jats:p>","DOI":"10.1002\/smll.202402492","type":"journal-article","created":{"date-parts":[[2024,8,7]],"date-time":"2024-08-07T10:53:21Z","timestamp":1723028001000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":18,"title":["Ni<sub>3<\/sub>C\/Ni<sub>3<\/sub>S<sub>2<\/sub> Heterojunction Electrocatalyst for Efficient Methanol Oxidation via Dual Anion Co\u2010modulation Strategy"],"prefix":"10.1002","volume":"20","author":[{"given":"Jin\u2010Gang\u2010Lu","family":"Tao","sequence":"first","affiliation":[{"name":"Key Laboratory for Advanced Materials and Institute of Fine Chemicals School of Chemistry and Molecular Engineering East China University of Science and Technology  130 Meilong Road Shanghai 200237 P. R. 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