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Although hydrophilic interfaces have long been regarded as favorable due to their strong water\u2013catalyst interactions, the molecular-level relationship between the interfacial water structure and hydrogen-evolution reactivity remains unclear. Here, we establish a direct structure\u2013reactivity correlation at the water\u2013TiO2 interface using a series of anatase TiO2 nanoparticle photocatalysts. By combining real-time mass spectrometry with infrared spectroscopy under precisely controlled hydration conditions ranging from sub-monolayer to multilayer regimes, we quantitatively evaluate intrinsic hydrogen-evolution activity per water layer and per unit surface area. We show that stronger water\u2013TiO2 interactions, characterized by higher adsorption energies and increased dissociative adsorption, correlate with lower H2 formation rates. Such strongly adsorbed water species form rigid hydrogen-bond networks that suppress interfacial water reactivity. In contrast, weaker water\u2013TiO2 interactions accompanied by soft and flexible hydrogen-bond networks promote photocatalytic H2 evolution more efficiently. These findings demonstrate that optimal photocatalytic performance arises not from maximizing hydrophilicity but from tuning interfaces toward more hydrophobic environments that support dynamically flexible hydrogen-bond networks. This study provides a molecular-level framework for rational interface design in photocatalytic hydrogen evolution.<\/jats:p>","DOI":"10.1021\/acs.jpclett.6c01721","type":"journal-article","created":{"date-parts":[[2026,9,5]],"date-time":"2026-09-05T03:02:02Z","timestamp":1788577322000},"page":"10708-10716","source":"Crossref","is-referenced-by-count":0,"title":["Bridging Interfacial\nWater Structure and Reactivity\nin Photocatalytic Hydrogen Evolution at TiO2 Interfaces"],"prefix":"10.1021","volume":"17","author":[{"ORCID":"https:\/\/orcid.org\/0000-0002-7602-1073","authenticated-orcid":true,"given":"Zhongqiu","family":"Lin","sequence":"first","affiliation":[{"name":"Institute for Molecular Science , , , ,","place":["Okazaki, Aichi, Japan, 444-8585"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-2845-5053","authenticated-orcid":true,"given":"Hikaru","family":"Saito","sequence":"additional","affiliation":[{"name":"Institute for Molecular Science , , , ,","place":["Okazaki, Aichi, Japan, 444-8585"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-3922-4581","authenticated-orcid":true,"given":"Hiromasa","family":"Sato","sequence":"additional","affiliation":[{"name":"Institute for Molecular Science , , , ,","place":["Okazaki, Aichi, Japan, 444-8585"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-3453-6009","authenticated-orcid":true,"given":"Toshiki","family":"Sugimoto","sequence":"additional","affiliation":[{"name":"Institute for Molecular Science , , , ,","place":["Okazaki, Aichi, Japan, 444-8585"]},{"name":"The Graduate University for Advanced Studies, SOKENDAI , , ,","place":["Okazaki, Aichi, Japan, 444-8585"]}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"316","published-online":{"date-parts":[[2026,9,4]]},"reference":[{"issue":"2","key":"2026091709082495500_cit1","doi-asserted-by":"publisher","first-page":"919","DOI":"10.1021\/acs.chemrev.9b00201","article-title":"Particulate\nPhotocatalysts for Light-Driven Water Splitting: Mechanisms,\nChallenges, and Design Strategies","volume":"120","author":"Wang","year":"2020","journal-title":"Chem. 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Interfaces"},{"issue":"2","key":"2026091709082495500_cit25","doi-asserted-by":"publisher","first-page":"100013","DOI":"10.1016\/j.xcrp.2019.100013","article-title":"Surface Water Loading on Titanium Dioxide Modulates Photocatalytic\nWater Splitting","volume":"1","author":"Yang","year":"2020","journal-title":"Cell Reports Phys. Sci."},{"issue":"32","key":"2026091709082495500_cit26","doi-asserted-by":"publisher","first-page":"22276","DOI":"10.1021\/jacs.4c04271","article-title":"Positive and Negative\nImpacts of Interfacial Hydrogen Bonds on Photocatalytic Hydrogen Evolution","volume":"146","author":"Lin","year":"2024","journal-title":"J. Am. Chem. Soc."},{"issue":"3","key":"2026091709082495500_cit27","doi-asserted-by":"publisher","first-page":"1790","DOI":"10.1021\/la2042873","article-title":"Water Adsorption\non Clay Minerals as a Function of\nRelative Humidity: Application of BET and Freundlich Adsorption Models","volume":"28","author":"Hatch","year":"2012","journal-title":"Langmuir"},{"issue":"2","key":"2026091709082495500_cit28","doi-asserted-by":"publisher","first-page":"1323","DOI":"10.1021\/acs.nanolett.5b04724","article-title":"Effect of\nWater Adsorption on Carrier Trapping Dynamics\nat the Surface of Anatase TiO2 Nanoparticles","volume":"16","author":"Shirai","year":"2016","journal-title":"Nano Lett."},{"issue":"36","key":"2026091709082495500_cit29","doi-asserted-by":"publisher","first-page":"24800","DOI":"10.1021\/jacs.3c14558","article-title":"Direct Operando Identification\nof Reactive Electron\nSpecies Driving Photocatalytic Hydrogen Evolution on Metal-Loaded\nOxides","volume":"146","author":"Sato","year":"2024","journal-title":"J. Am. Chem. Soc."},{"issue":"2\u20133","key":"2026091709082495500_cit30","doi-asserted-by":"publisher","first-page":"433","DOI":"10.1016\/j.cej.2010.11.093","article-title":"Production of Peroxide Species in\nPt\/TiO2 Suspensions under Conditions of Photocatalytic\nWater Splitting and Glycerol Photoreforming","volume":"170","author":"Daskalaki","year":"2011","journal-title":"Chem. Eng. J."},{"key":"2026091709082495500_cit31","doi-asserted-by":"publisher","first-page":"291","DOI":"10.1038\/s41929-018-0055-z","article-title":"Identifying\nthe Key Obstacle in Photocatalytic Oxygen Evolution on Rutile TiO2","volume":"1","author":"Wang","year":"2018","journal-title":"Nat. Catal."},{"issue":"26","key":"2026091709082495500_cit32","doi-asserted-by":"publisher","first-page":"18061","DOI":"10.1021\/jacs.4c05042","article-title":"Water Structure\nin the First Layers on TiO2: A Key Factor for Boosting\nSolar-Driven Water-Splitting Performances","volume":"146","author":"Verduci","year":"2024","journal-title":"J.\nAm. Chem. Soc."},{"issue":"35","key":"2026091709082495500_cit33","doi-asserted-by":"publisher","first-page":"29943","DOI":"10.1021\/acsami.8b08172","article-title":"Curved TiO2 Nanoparticles\nin Water: Short (Chemical) and Long (Physical)\nRange Interfacial Effects","volume":"10","author":"Fazio","year":"2018","journal-title":"ACS Appl. Mater.\nInterfaces"},{"key":"2026091709082495500_cit34","doi-asserted-by":"publisher","first-page":"066107","DOI":"10.1103\/PhysRevLett.96.066107","article-title":"Formation and Splitting\nof Paired Hydroxyl Groups on Reduced TiO2(110)","volume":"96","author":"Wendt","year":"2006","journal-title":"Phys. Rev. Lett."},{"issue":"48","key":"2026091709082495500_cit35","doi-asserted-by":"publisher","first-page":"41319","DOI":"10.1021\/acsnano.5c15817","article-title":"Positive Impact of\nWeak Hydrogen Bonds on O\u2013H Bond Dissociation in Photocatalytic\nWater Splitting","volume":"19","author":"Li","year":"2025","journal-title":"ACS Nano"},{"key":"2026091709082495500_cit36","doi-asserted-by":"publisher","first-page":"1220","DOI":"10.1063\/1.447808","article-title":"The Uncoupled O\u2013H\nStretch in Ice VII. The Infrared\nFrequency and Integrated Intensity up to 189 kbar","volume":"81","author":"Klug","year":"1984","journal-title":"J. Chem. Phys."},{"key":"2026091709082495500_cit37","doi-asserted-by":"publisher","first-page":"5323","DOI":"10.1063\/1.452557","article-title":"High-Density Amorphous Ice. IV. Raman\nSpectrum of the Uncoupled O\u2013H and O\u2013D Oscillators","volume":"86","author":"Klug","year":"1987","journal-title":"J. Chem. 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Solution Chem."},{"issue":"2","key":"2026091709082495500_cit41","doi-asserted-by":"publisher","first-page":"213","DOI":"10.1016\/j.vibspec.2009.05.002","article-title":"The Raman\nOH Stretching Bands of Liquid Water","volume":"51","author":"Sun","year":"2009","journal-title":"Vib. Spectrosc."},{"issue":"16","key":"2026091709082495500_cit42","doi-asserted-by":"publisher","first-page":"3005","DOI":"10.1039\/b506641g","article-title":"The Effect\nof Cooperative Hydrogen Bonding on the OH Stretching-Band Shift for\nWater Clusters Studied by Matrix-Isolation Infrared Spectroscopy and\nDensity Functional Theory","volume":"7","author":"Ohno","year":"2005","journal-title":"Phys. Chem. Chem.\nPhys."},{"issue":"35","key":"2026091709082495500_cit43","doi-asserted-by":"publisher","first-page":"20735","DOI":"10.1021\/acs.jpcc.5b06384","article-title":"Spherical versus Faceted Anatase\nTiO2 Nanoparticles: A Model Study of Structural and Electronic\nProperties","volume":"119","author":"Fazio","year":"2015","journal-title":"J. Phys. Chem. C"},{"key":"2026091709082495500_cit44","doi-asserted-by":"publisher","first-page":"177","DOI":"10.1007\/BFb0116438","article-title":"Hydrogen Bonding\nin Solids. Correlation of Spectroscopic and Crystallographic Data","volume":"18","author":"Novak","year":"1974","journal-title":"Struct. Bonding (Berlin)"},{"key":"2026091709082495500_cit45","doi-asserted-by":"publisher","first-page":"211","DOI":"10.1016\/0167-5729(87)90001-X","article-title":"The Interaction\nof Water with Solid Surfaces: Fundamental\nAspects","volume":"7","author":"Thiel","year":"1987","journal-title":"Surf. Sci. Rep."},{"issue":"19","key":"2026091709082495500_cit46","doi-asserted-by":"publisher","first-page":"9919","DOI":"10.1021\/cr5001892","article-title":"Understanding\nTiO2 photocatalysis:\nMechanisms and Materials","volume":"114","author":"Schneider","year":"2014","journal-title":"Chem. Rev."},{"issue":"20","key":"2026091709082495500_cit47","doi-asserted-by":"publisher","first-page":"5905","DOI":"10.1002\/anie.201412035","article-title":"Activation of Water\nin Titanium Dioxide\nPhotocatalysis by Formation of Surface Hydrogen Bonds: An in Situ\nIR Spectroscopy Study","volume":"54","author":"Sheng","year":"2015","journal-title":"Angew. Chemie - Int.\nEd."},{"issue":"30","key":"2026091709082495500_cit48","doi-asserted-by":"publisher","first-page":"13565","DOI":"10.1021\/jacs.2c03690","article-title":"Hydrogen-Bond Network Promotes Water\nSplitting on the TiO2 Surface","volume":"144","author":"Ma","year":"2022","journal-title":"J.\nAm. Chem. Soc."},{"issue":"4","key":"2026091709082495500_cit49","doi-asserted-by":"publisher","first-page":"2002","DOI":"10.1021\/jacs.1c13250","article-title":"Pathways for Electron Transfer at\nMgO-Water Interfaces from Ab Initio Molecular Dynamics","volume":"144","author":"Ding","year":"2022","journal-title":"J. Am. Chem. Soc."},{"issue":"16","key":"2026091709082495500_cit50","doi-asserted-by":"publisher","first-page":"3998","DOI":"10.1021\/acs.jpcb.4c07371","article-title":"Hydration\nWater Dynamics in Zwitterionic Phospholipid Membranes Mixed with Charged\nPhospholipids","volume":"129","author":"Rahman","year":"2025","journal-title":"J. Phys. Chem. B"},{"issue":"39","key":"2026091709082495500_cit51","doi-asserted-by":"publisher","first-page":"15077","DOI":"10.1021\/jp037584m","article-title":"Particle-Size-Dependent Distribution of Carboxylate Adsorption Sites\non TiO2 Nanoparticle Surfaces: Insights into the Surface\nModification of Nanostructured TiO2 Electrodes","volume":"108","author":"Zhang","year":"2004","journal-title":"J. Phys. Chem. B"},{"key":"2026091709082495500_cit52","doi-asserted-by":"publisher","first-page":"4378","DOI":"10.1038\/s41467-018-06917-4","article-title":"Effect of\nHydrophobic Cations on the Oxygen Reduction Reaction on Single\u2013crystal\nPlatinum Electrodes","volume":"9","author":"Kumeda","year":"2018","journal-title":"Nat. Commun."}],"container-title":["The Journal of Physical\nChemistry Letters"],"original-title":[],"language":"en","link":[{"URL":"https:\/\/pubs.acs.org\/doi\/pdf\/10.1021\/acs.jpclett.6c01721","content-type":"application\/pdf","content-version":"vor","intended-application":"unspecified"},{"URL":"https:\/\/pubs.acs.org\/jpclcd\/article-pdf\/17\/37\/10708\/68394830\/acs.jpclett.6c01721.pdf","content-type":"application\/pdf","content-version":"vor","intended-application":"syndication"},{"URL":"https:\/\/pubs.acs.org\/jpclcd\/article-pdf\/17\/37\/10708\/68394830\/acs.jpclett.6c01721.pdf","content-type":"unspecified","content-version":"vor","intended-application":"similarity-checking"}],"deposited":{"date-parts":[[2026,9,17]],"date-time":"2026-09-17T14:04:07Z","timestamp":1789653847000},"score":1,"resource":{"primary":{"URL":"https:\/\/pubs.acs.org\/jpclcd\/article\/17\/37\/10708\/5421828\/Bridging-Interfacial-Water-Structure-and"}},"subtitle":[],"short-title":[],"issued":{"date-parts":[[2026,9,4]]},"references-count":52,"journal-issue":{"issue":"37","published-online":{"date-parts":[[2026,9,4]]},"published-print":{"date-parts":[[2026,9,17]]}},"URL":"https:\/\/doi.org\/10.1021\/acs.jpclett.6c01721","relation":{},"ISSN":["1948-7185"],"issn-type":[{"value":"1948-7185","type":"electronic"}],"subject":[],"published":{"date-parts":[[2026,9,4]]}}}