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Here, to realize PQD\u2010catalyzed photocatalytic N<jats:sub>2<\/jats:sub> reduction reaction (NRR), water\u2010resistant PQDs are simply prepared through one\u2010step electrospray synthesis in microseconds. During the fast electrospray, PQDs of Zn\/PbO\u2010doped methylammonium lead bromide (Zn\/PbO\/PC\u2013Zn\/MAPbBr<jats:sub>3<\/jats:sub>, MA: CH<jats:sub>3<\/jats:sub>NH<jats:sub>3<\/jats:sub>) are prepared and part\u2010encapsulated by polycarbonate. The synthesis maintains good water resistance, whose restriction on charge transport is overcome skillfully. Simultaneously, substitution of Zn with Pb on water\u2010resistant surface is also achieved, which fabricates new Zn\u2013oxygen vacancies (Zn\u2010OVs) with Zn\/PbO\u2013Zn\/MAPbBr<jats:sub>3<\/jats:sub> type I heterojunction. This facilitates efficient electron transfer from internal heterojunction interface of Zn\/MAPbBr<jats:sub>3<\/jats:sub> PQDs to the surface of Zn\/PbO. Demonstrated by theoretical calculations, Zn\u2010OVs promote chemisorption and polarization of N<jats:sub>2<\/jats:sub>. In addition, s\u2010electrons in exposed Zn become active due to changes of electron filling of Zn orbitals under OVs\u2019 co\u2010doping. Thus, photocatalytic N<jats:sub>2<\/jats:sub> reduction reaction catalyzed by organic\u2013inorganic hybrid PQDs is first achieved in aqueous phase without sacrificial agents being added. This initiates possibilities for photocatalytic applications of organic\u2013inorganic hybrid PQDs in aqueous phase.<\/jats:p>","DOI":"10.1002\/smll.202103773","type":"journal-article","created":{"date-parts":[[2021,10,5]],"date-time":"2021-10-05T11:10:00Z","timestamp":1633432200000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":18,"title":["One\u2010Step Prepared Water\u2010Resistant Organic\u2013Inorganic\u2010Hybrid Perovskite Quantum Dots with Zn\u2013Oxygen Vacancies for Attempts at Nitrogen Fixation"],"prefix":"10.1002","volume":"17","author":[{"given":"Yixuan","family":"Gao","sequence":"first","affiliation":[{"name":"Key Laboratory of Radiopharmaceuticals Key Laboratory of Theoretical and Computational Photochemistry College of Chemistry Beijing Normal University  No.19, Xinjiekouwai Street, Haidian District Beijing 100875 P. R. 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