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While the functionality of single\u2010metal catalysts is relatively well\u2010understood, the mechanism and synergy of bimetallic systems are less explored. Herein, the design and fabrication of an integrated flexible electrode based on NiCo<jats:sub>2<\/jats:sub>S<jats:sub>4<\/jats:sub>\/graphitic carbon nitride\/carbon nanotube (NiCo<jats:sub>2<\/jats:sub>S<jats:sub>4<\/jats:sub>@g\u2010C<jats:sub>3<\/jats:sub>N<jats:sub>4<\/jats:sub>\u2010CNT) are reported. Comparative studies evidence the electronic transfer from bimetallic Ni\/Co active sites to abundant pyridinic\u2010N in underlying g\u2010C<jats:sub>3<\/jats:sub>N<jats:sub>4<\/jats:sub> and the synergistic effect with coupled conductive CNTs for promoting reversible oxygen electrocatalysis. Theoretical calculations demonstrate the unique coactivation of bimetallic Ni\/Co atoms by pyridinic\u2010N species (a Ni, Co\u2013N<jats:sub>2<\/jats:sub> moiety), which simultaneously downshifts their d\u2010band center positions and benefits the adsorption\/desorption features of oxygen intermediates, accelerating the reaction kinetics. The optimized NiCo<jats:sub>2<\/jats:sub>S<jats:sub>4<\/jats:sub>@g\u2010C<jats:sub>3<\/jats:sub>N<jats:sub>4<\/jats:sub>\u2010CNT hybrid manifests outstanding bifunctional performance for catalyzing oxygen reduction\/evolution reactions, highly efficient for realistic zinc\u2013air batteries featuring low overpotential, high efficiency, and long durability, superior to those of physical mixed counterparts and state\u2010of\u2010the\u2010art noble metal catalysts. The identified bimetallic coactivation mechanism will shed light on the rational design and interfacial engineering of hybrid nanomaterials for diverse applications.<\/jats:p>","DOI":"10.1002\/adma.201808281","type":"journal-article","created":{"date-parts":[[2019,3,15]],"date-time":"2019-03-15T03:31:06Z","timestamp":1552620666000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":379,"title":["Identifying the Activation of Bimetallic Sites in NiCo<sub>2<\/sub>S<sub>4<\/sub>@g\u2010C<sub>3<\/sub>N<sub>4<\/sub>\u2010CNT Hybrid Electrocatalysts for Synergistic Oxygen Reduction and Evolution"],"prefix":"10.1002","volume":"31","author":[{"given":"Xiaopeng","family":"Han","sequence":"first","affiliation":[{"name":"School of Materials Science and Engineering Tianjin Key Laboratory of Composite and Functional Materials Key Laboratory of Advanced Ceramics and Machining Technology (Ministry of Education) Tianjin University  Tianjin 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Laboratory of Advanced Ceramics and Machining Technology (Ministry of Education) Tianjin University  Tianjin 300072 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Naiqin","family":"Zhao","sequence":"additional","affiliation":[{"name":"School of Materials Science and Engineering Tianjin Key Laboratory of Composite and Functional Materials Key Laboratory of Advanced Ceramics and Machining Technology (Ministry of Education) Tianjin University  Tianjin 300072 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Wenbin","family":"Hu","sequence":"additional","affiliation":[{"name":"School of Materials Science and Engineering Tianjin Key Laboratory of Composite and Functional Materials Key Laboratory of Advanced Ceramics and Machining Technology (Ministry of Education) Tianjin University  Tianjin 300072 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