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In this work, we systematically investigate aperture\u2010size\u2010controlled hot\u2010carrier transfer and mass transport coupling in gold nanocups (AuNCs) with precisely tuned cavity diameters (35\u201367\u00a0nm). Single\u2010particle catalytic imaging reveals that AuNCs with a medium aperture size (\u224858\u00a0nm) exhibit optimal photocatalytic activity, achieving a maximum turnover rate of 0.59 \u00b1 0.007 s\n                    <jats:sup>\u22121<\/jats:sup>\n                    , 2.8\u20138.4\u2010fold higher than extreme\u2010aperture variants. Theoretic simulations correlate this enhancement with intensified electric field localization (|\n                    <jats:italic>E<\/jats:italic>\n                    <jats:sub>max<\/jats:sub>\n                    |\/|\n                    <jats:italic>E<\/jats:italic>\n                    <jats:sub>0<\/jats:sub>\n                    | = 5.1) and hot\u2010carrier generation at the cup rim, while kinetic analysis identifies dominant substrate\u2010assisted desorption (\n                    <jats:italic>k<\/jats:italic>\n                    <jats:sub>2<\/jats:sub>\n                    = 6.12 \u00b1 0.14 s\n                    <jats:sup>\u22121<\/jats:sup>\n                    ) and strong spatiotemporal memory effect. The work deciphers the synergy between electromagnetic confinement and molecular transport at the single\u2010particle level, demonstrating that cavity geometry governs reactant adsorption, product desorption pathways, and active\u2010site stability. These findings establish a geometric design principle for plasmonic photocatalysts, advancing the rational engineering of high\u2010efficiency solar\u2010to\u2010chemical conversion systems for sustainable energy applications.\n                  <\/jats:p>","DOI":"10.1002\/smll.202514585","type":"journal-article","created":{"date-parts":[[2026,2,18]],"date-time":"2026-02-18T19:28:08Z","timestamp":1771442888000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":2,"title":["Single\u2010Particle Kinetics Unravel Aperture\u2010Size Dominance in Hot\u2010Carrier Transfer and Product Desorption for Photocatalytic Reactions in Plasmonic Nanocavities"],"prefix":"10.1002","volume":"22","author":[{"given":"Lin","family":"Wei","sequence":"first","affiliation":[{"name":"Key Laboratory of Chemical Biology and Traditional Chinese Medicine Research National and Local Joint Engineering Laboratory for New Petrochemical Materials and Fine Utilization of Resources College of Chemistry and Chemical Engineering Hunan Normal University  Changsha China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Jie","family":"Yang","sequence":"additional","affiliation":[{"name":"Key Laboratory of Chemical Biology and Traditional Chinese Medicine Research National and Local Joint Engineering Laboratory for New Petrochemical Materials and Fine Utilization of Resources College of Chemistry and Chemical Engineering Hunan Normal University  Changsha China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Yanan","family":"Deng","sequence":"additional","affiliation":[{"name":"College of Chemistry and Chemical Engineering Central South University  Changsha China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Xiulin","family":"Fan","sequence":"additional","affiliation":[{"name":"College of Chemistry and Chemical Engineering Central South University  Changsha China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Chen","family":"Zhang","sequence":"additional","affiliation":[{"name":"College of Chemistry and Chemical Engineering Central South University  Changsha China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Zhongju","family":"Ye","sequence":"additional","affiliation":[{"name":"College of Chemistry Zhengzhou University  Zhengzhou China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-0522-2342","authenticated-orcid":false,"given":"Lehui","family":"Xiao","sequence":"additional","affiliation":[{"name":"College of Chemistry and Chemical Engineering Central South University  Changsha 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