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Here an oxygen\u2010coordinated nickel single\u2010atom catalyst (Ni\u2013O\u2013C) is reported with bifunctional electrocatalytic activities toward the two\u2010electron oxygen reduction reaction (2e<jats:sup>\u2212<\/jats:sup> ORR) to H<jats:sub>2<\/jats:sub>O<jats:sub>2<\/jats:sub> and H<jats:sub>2<\/jats:sub>O<jats:sub>2<\/jats:sub>\u2010assisted benzene oxidation to phenol. The Ni\u2013(O\u2013C<jats:sub>2<\/jats:sub>)<jats:sub>4<\/jats:sub> sites in Ni\u2013O\u2013C ar proven to be the catalytic active centers for bifunctional 2e<jats:sup>\u2212<\/jats:sup> ORR and H<jats:sub>2<\/jats:sub>O<jats:sub>2<\/jats:sub>\u2010assisted benzene oxidation processes. As a result, Ni\u2013O\u2013C can afford a benzene conversion as high as 96.4 \u00b1 3.6% with a phenol selectivity of 100% and a Faradaic efficiency (FE) of 80.2 \u00b1 3.2% with the help of H<jats:sub>2<\/jats:sub>O<jats:sub>2<\/jats:sub> in 0.1\u00a0<jats:sc>m<\/jats:sc> KOH electrolyte at 1.5\u00a0V (vs RHE). A proof of concept experiment with Ni\u2013O\u2013C concurrently as cathode and anode in a single electrochemical cell demonstrates a benzene conversion of 33.4 \u00b1 2.2% with a phenol selectivity of 100% and a FE of 44.8 \u00b1 3.0% at 10\u00a0mA cm<jats:sup>\u22122<\/jats:sup>.<\/jats:p>","DOI":"10.1002\/advs.202204043","type":"journal-article","created":{"date-parts":[[2022,10,30]],"date-time":"2022-10-30T23:21:50Z","timestamp":1667172110000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":19,"title":["Hydrogen Peroxide Assisted Electrooxidation of Benzene to Phenol over Bifunctional Ni\u2013(O\u2013C<sub>2<\/sub>)<sub>4<\/sub> Sites"],"prefix":"10.1002","volume":"9","author":[{"given":"Shengbo","family":"Zhang","sequence":"first","affiliation":[{"name":"Key Laboratory of Materials Physics Centre for Environmental and Energy Nanomaterials Anhui Key Laboratory of Nanomaterials and Nanotechnology CAS Center for Excellence 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