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TiO<jats:sub>2<\/jats:sub>, a widely employed photocatalyst, typically stabilizes single atoms at oxygen vacancies\u2014sites that are accessible but prone to agglomeration under illumination. Here, we demonstrate that cation vacancies in Ti\u2010deficient TiO<jats:sub>2<\/jats:sub> nanosheets provide highly stable anchoring sites for Pt single atoms, enabling persistent photocatalytic hydrogen evolution. Ultrathin TiO<jats:sub>2<\/jats:sub> nanosheets with intrinsic Ti<jats:sup>4+<\/jats:sup> vacancies are synthesized via lepidocrocite\u2010type titanate delamination and Pt single atoms are selectively trapped within these vacancies through a simple immersion process. The resulting Pt\u2010decorated nanosheets exhibit superior photocatalytic hydrogen evolution performance, outperforming both Pt nanoparticle\u2010loaded nanosheets and benchmarked Pt single\u2010atom catalysts on P25. Crucially, Pt atoms anchored at Ti<jats:sup>4+<\/jats:sup> vacancies display remarkable resistance to light\u2010induced agglomeration, a key limitation of conventional single\u2010atom photocatalysts. Density functional theory calculations reveal that Pt incorporation into Ti<jats:sup>4+<\/jats:sup> vacancies is highly thermodynamically favorable and optimizes hydrogen adsorption energetics for enhanced catalytic activity. This work highlights the critical role of cation defect engineering in stabilizing single\u2010atom co\u2010catalysts and advancing the efficiency and durability of photocatalytic hydrogen evolution.<\/jats:p>","DOI":"10.1002\/smll.202502428","type":"journal-article","created":{"date-parts":[[2025,6,2]],"date-time":"2025-06-02T09:19:47Z","timestamp":1748855987000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":18,"title":["Cation Vacancies in Ti\u2010Deficient TiO<sub>2<\/sub> Nanosheets Enable Highly Stable Trapping of Pt Single Atoms for Persistent Photocatalytic Hydrogen Evolution"],"prefix":"10.1002","volume":"21","author":[{"given":"Hayoon","family":"Jung","sequence":"first","affiliation":[{"name":"Department of Materials Science and Engineering WW4\u2010LKO Friedrich\u2010Alexander\u2010Universit\u00e4t Erlangen\u2010N\u00fcrnberg  Martensstra\u00dfe 7 91058 Erlangen Germany"},{"name":"Regional Centre of Advanced Technologies and Materials Czech Advanced Technology and Research Institute (CATRIN) Palack\u00fd University  \u0160lechtitel\u016f 27 Olomouc 78371 Czech Republic"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Gihoon","family":"Cha","sequence":"additional","affiliation":[{"name":"Department for Correlative Microscopy and Materials Data Fraunhofer Institute for Ceramic Technologies and Systems (IKTS)  \u00c4u\u00dfere N\u00fcrnberger Stra\u00dfe 62 91301 Forchheim Germany"},{"name":"Department of Chemistry Universit\u00e4t Bayreuth  Universit\u00e4tsstra\u00dfe 30 95447 Bayreuth Germany"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Hyesung","family":"Kim","sequence":"additional","affiliation":[{"name":"Department of Materials Science and Engineering WW4\u2010LKO Friedrich\u2010Alexander\u2010Universit\u00e4t Erlangen\u2010N\u00fcrnberg  Martensstra\u00dfe 7 91058 Erlangen Germany"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Johannes","family":"Will","sequence":"additional","affiliation":[{"name":"Institute of Micro\u2010 and Nanostructure Research &amp; 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