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However, direct nanoscale visualization of microdroplet-regulated interfacial reaction pathways remains a fundamental challenge. Herein, we report a tip-enhanced Raman spectroscopy (TERS) approach to probe and visualize competing surface reactions induced by microdroplets at the nanometer scale using a model system consisting of 4-mercaptophenylboronic acid (4-MPBA) on Au(111). By coupling TERS with controlled microdroplet treatments, we identify and spatially resolve two competing surface reaction pathways: EF-mediated covalent condensation and \u00b7OH-mediated oxidation. Density functional theory (DFT) calculations and radical scavenging experiments provide additional support for the proposed reaction mechanism. Systematic modulation of the interfacial EF strength and \u00b7OH abundance enables precise control over the product distribution, as revealed by high-resolution TERS imaging. Our results demonstrate that TERS provides an exceptional platform for mapping microdroplet-regulated interfacial reaction pathways, opening new avenues for mechanistic studies and reaction control in confined interfacial environments.<\/jats:p>","DOI":"10.1021\/acs.analchem.6c02622","type":"journal-article","created":{"date-parts":[[2026,8,20]],"date-time":"2026-08-20T23:50:03Z","timestamp":1787269803000},"page":"25013-25021","source":"Crossref","is-referenced-by-count":0,"title":["Nanoscale Visualization\nof Microdroplet-Regulated\nInterfacial Reaction Pathways by Tip-Enhanced Raman Spectroscopy"],"prefix":"10.1021","volume":"98","author":[{"given":"Yue-Wen","family":"Zhou","sequence":"first","affiliation":[{"name":"Sichuan University , , 29 Wangjiang Road , ,","place":["Chengdu, P. R. China, 610064"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Ming-Yang","family":"Jia","sequence":"additional","affiliation":[{"name":"Sichuan University , , 29 Wangjiang Road , ,","place":["Chengdu, P. R. China, 610064"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0009-0005-5890-1981","authenticated-orcid":true,"given":"Qinlei","family":"Liu","sequence":"additional","affiliation":[{"name":"Sichuan University , , 29 Wangjiang Road , ,","place":["Chengdu, P. R. China, 610064"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-1659-4291","authenticated-orcid":true,"given":"Zhen-Feng","family":"Cai","sequence":"additional","affiliation":[{"name":"Sichuan University , , 29 Wangjiang Road , ,","place":["Chengdu, P. R. China, 610064"]}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"316","published-online":{"date-parts":[[2026,8,20]]},"reference":[{"issue":"19","key":"2026090306460659300_cit1","doi-asserted-by":"publisher","first-page":"16060","DOI":"10.1021\/jacs.4c17760","article-title":"Microdroplet Cascade Catalysis for\nHighly Selective Production of Propylene Glycol under Ambient Conditions","volume":"147","author":"Dong","year":"2025","journal-title":"J. Am. Chem. Soc."},{"issue":"23","key":"2026090306460659300_cit2","doi-asserted-by":"publisher","first-page":"19595","DOI":"10.1021\/jacs.5c00720","article-title":"Microdroplet\nSurface Drives and Accelerates\nProton-Controlled, Size-Dependent Nitrate Photolysis","volume":"147","author":"Zhang","year":"2025","journal-title":"J. Am. Chem. Soc."},{"issue":"15","key":"2026090306460659300_cit3","doi-asserted-by":"publisher","first-page":"10963","DOI":"10.1021\/jacs.4c02312","article-title":"Deciphering the Microdroplet Acceleration\nFactors of Aza-Michael Addition Reactions","volume":"146","author":"Song","year":"2024","journal-title":"J.\nAm. Chem. Soc."},{"issue":"48","key":"2026090306460659300_cit4","doi-asserted-by":"publisher","first-page":"26003","DOI":"10.1021\/jacs.3c11650","article-title":"Harnessing\nthe High Interfacial Electric\nFields on Water Microdroplets to Accelerate Menshutkin Reactions","volume":"145","author":"Song","year":"2023","journal-title":"J. Am. Chem. Soc."},{"issue":"50","key":"2026090306460659300_cit5","doi-asserted-by":"publisher","first-page":"27198","DOI":"10.1021\/jacs.3c08643","article-title":"Water Microdroplets-Initiated\nMethane\nOxidation","volume":"145","author":"Song","year":"2023","journal-title":"J. Am. Chem. 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Phys."},{"issue":"35","key":"2026090306460659300_cit26","doi-asserted-by":"publisher","first-page":"24389","DOI":"10.1021\/jacs.4c06171","article-title":"Enhanced Selectivity in Microdroplet-Mediated\nEnzyme Catalysis","volume":"146","author":"Li","year":"2024","journal-title":"J. Am. Chem. Soc."},{"issue":"5","key":"2026090306460659300_cit27","doi-asserted-by":"publisher","first-page":"756","DOI":"10.1038\/s41557-025-01762-7","article-title":"Aging-dependent\nevolving electrochemical potentials of biomolecular condensates regulate\ntheir physicochemical activities","volume":"17","author":"Yu","year":"2025","journal-title":"Nat. Chem."},{"issue":"6","key":"2026090306460659300_cit28","doi-asserted-by":"publisher","first-page":"1594","DOI":"10.1016\/j.chempr.2023.04.001","article-title":"Interface of biomolecular condensates modulates redox\nreactions","volume":"9","author":"Dai","year":"2023","journal-title":"Chem"},{"issue":"3","key":"2026090306460659300_cit29","doi-asserted-by":"publisher","first-page":"2227","DOI":"10.1021\/jacs.3c12586","article-title":"Charged Microdroplets as Microelectrochemical\nCells\nfor CO2 Reduction and C\u2013C Coupling","volume":"146","author":"Dong","year":"2024","journal-title":"J. Am. Chem. Soc."},{"issue":"1","key":"2026090306460659300_cit30","doi-asserted-by":"publisher","first-page":"228","DOI":"10.1007\/s11244-021-01418-z","article-title":"What Role Does the\nElectric Double Layer Play in Redox\nReactions at Planar Electrostatically Charged Insulating Surfaces?","volume":"65","author":"Chamberlayne","year":"2022","journal-title":"Top. Catal."},{"issue":"19","key":"2026090306460659300_cit31","doi-asserted-by":"publisher","first-page":"8302","DOI":"10.1021\/acs.jpclett.0c02247","article-title":"Effects of Weak\nElectrolytes on Electric\nDouble Layer Ion Distributions","volume":"11","author":"Chamberlayne","year":"2020","journal-title":"J. Phys. Chem.\nLett."},{"issue":"4","key":"2026090306460659300_cit32","doi-asserted-by":"publisher","first-page":"1169","DOI":"10.1038\/s41596-019-0132-z","article-title":"Nanoscale\nchemical\nimaging using tip-enhanced Raman spectroscopy","volume":"14","author":"Kumar","year":"2019","journal-title":"Nat. Protoc."},{"issue":"1","key":"2026090306460659300_cit33","doi-asserted-by":"publisher","first-page":"55","DOI":"10.31635\/ccschem.022.202202287","article-title":"Probing On-Surface\nChemistry at the\nNanoscale Using Tip-Enhanced Raman Spectroscopy","volume":"5","author":"Cai","year":"2023","journal-title":"CCS Chem."},{"issue":"3","key":"2026090306460659300_cit34","doi-asserted-by":"publisher","first-page":"963","DOI":"10.1039\/D2NR05127C","article-title":"Nanoscale\nchemical analysis of 2D\nmolecular materials using tip-enhanced Raman spectroscopy","volume":"15","author":"Mr\u0111enovic\u0301","year":"2023","journal-title":"Nanoscale"},{"issue":"1","key":"2026090306460659300_cit35","doi-asserted-by":"publisher","first-page":"3305","DOI":"10.1021\/acsami.5c23749","article-title":"Interfacial-Environment-Regulated\nRadical Pathways in Plasma-Induced C\u2013X Bond Transformation","volume":"18","author":"Yang","year":"2026","journal-title":"ACS Appl. Mater. Interfaces"},{"issue":"38","key":"2026090306460659300_cit36","doi-asserted-by":"publisher","first-page":"15624","DOI":"10.1021\/jacs.1c04380","article-title":"Angstrom-Scale Spectroscopic\nVisualization of Interfacial Interactions in an Organic\/Borophene\nVertical Heterostructure","volume":"143","author":"Li","year":"2021","journal-title":"J. Am. Chem. Soc."},{"issue":"1","key":"2026090306460659300_cit37","doi-asserted-by":"publisher","first-page":"1796","DOI":"10.1038\/s41467-022-29445-8","article-title":"Chemically\nidentifying single adatoms with single-bond sensitivity\nduring oxidation reactions of borophene","volume":"13","author":"Li","year":"2022","journal-title":"Nat.\nCommun."},{"issue":"7","key":"2026090306460659300_cit38","doi-asserted-by":"publisher","first-page":"1961","DOI":"10.1021\/acs.jpclett.1c00074","article-title":"Raman Detection of Bond Breaking\nand Making of a Chemisorbed Up-Standing Single Molecule at Single-Bond\nLevel","volume":"12","author":"Wang","year":"2021","journal-title":"J. Phys. Chem. Lett."},{"issue":"1","key":"2026090306460659300_cit39","doi-asserted-by":"publisher","first-page":"538","DOI":"10.1021\/jacs.1c11263","article-title":"Molecular-Level Insights on Reactive\nArrangement in On-Surface Photocatalytic Coupling Reactions Using\nTip-Enhanced Raman Spectroscopy","volume":"144","author":"Cai","year":"2022","journal-title":"J. Am. Chem.\nSoc."},{"issue":"6531","key":"2026090306460659300_cit40","doi-asserted-by":"publisher","first-page":"818","DOI":"10.1126\/science.abd1827","article-title":"Determining\nstructural and chemical heterogeneities of surface species at the\nsingle-bond limit","volume":"371","author":"Xu","year":"2021","journal-title":"Science"},{"issue":"10","key":"2026090306460659300_cit41","doi-asserted-by":"publisher","first-page":"834","DOI":"10.1038\/s41929-020-00511-y","article-title":"Nanometre-scale spectroscopic\nvisualization of catalytic sites during a hydrogenation reaction on\na Pd\/Au bimetallic catalyst","volume":"3","author":"Yin","year":"2020","journal-title":"Nat. Catal."},{"issue":"6","key":"2026090306460659300_cit42","doi-asserted-by":"publisher","first-page":"6511","DOI":"10.1021\/acsnano.4c17728","article-title":"Monitoring\nthe On-Surface Boronic Acid Condensation Process at the Nanoscale\nUsing Tip-Enhanced Raman Spectroscopy","volume":"19","author":"Xia","year":"2025","journal-title":"ACS Nano"},{"issue":"10","key":"2026090306460659300_cit43","doi-asserted-by":"publisher","first-page":"865","DOI":"10.1038\/nnano.2015.170","article-title":"Distinguishing adjacent\nmolecules on a surface using plasmon-enhanced Raman scattering","volume":"10","author":"Jiang","year":"2015","journal-title":"Nat. Nanotechnol."},{"issue":"31","key":"2026090306460659300_cit44","doi-asserted-by":"publisher","first-page":"12380","DOI":"10.1021\/jacs.1c06366","article-title":"Molecular-Scale Chemical\nImaging of the Orientation of an On-Surface Coordination Complex by\nTip-Enhanced Raman Spectroscopy","volume":"143","author":"Cai","year":"2021","journal-title":"J. Am. Chem.\nSoc."},{"key":"2026090306460659300_cit45","doi-asserted-by":"publisher","first-page":"698","DOI":"10.1016\/j.saa.2013.11.109","article-title":"Vibrational\nspectroscopy and density functional theory study of 4-mercaptophenol","volume":"122","author":"Li","year":"2014","journal-title":"Spectrochim. Acta, A"},{"issue":"19","key":"2026090306460659300_cit46","doi-asserted-by":"publisher","first-page":"8470","DOI":"10.1039\/D5SC01466B","article-title":"Electric-field-induced\ncovalent condensation of boronic acids in water microdroplets","volume":"16","author":"Zhou","year":"2025","journal-title":"Chem. Sci."},{"issue":"49","key":"2026090306460659300_cit47","doi-asserted-by":"publisher","first-page":"30934","DOI":"10.1073\/pnas.2020158117","article-title":"Condensing\nwater vapor to droplets\ngenerates hydrogen peroxide","volume":"117","author":"Lee","year":"2020","journal-title":"Proc. Natl. Acad.\nSci. U. S. A."},{"issue":"11","key":"2026090306460659300_cit48","doi-asserted-by":"publisher","first-page":"4488","DOI":"10.1021\/jacsau.4c00810","article-title":"Stabilizing Highly\nReactive Aryl Carbanions in Water Microdroplets: Electrophilic Ipso-Substitution\nat the Air\u2013Water Interface","volume":"4","author":"Nandy","year":"2024","journal-title":"JACS Au"},{"issue":"35","key":"2026090306460659300_cit49","doi-asserted-by":"publisher","first-page":"19202","DOI":"10.1021\/jacs.3c08638","article-title":"Catalyst-Free Formation of Phenol\nfrom Benzoic Acid Using Water Microdroplets","volume":"145","author":"Meng","year":"2023","journal-title":"J. Am. Chem. Soc."},{"issue":"6","key":"2026090306460659300_cit50","doi-asserted-by":"publisher","DOI":"10.1002\/anie.202316131","article-title":"Superfast\nFormation of C(sp2)\u2013N, C(sp2)\u2013P,\nand C(sp2)\u2013S\nVinylic Bonds in Water Microdroplets","volume":"63","author":"Meng","year":"2024","journal-title":"Angew.\nChem., Int. Ed."},{"issue":"5","key":"2026090306460659300_cit51","doi-asserted-by":"publisher","first-page":"1036","DOI":"10.1007\/s13361-018-1908-z","article-title":"Microdroplets Accelerate\nRing Opening of Epoxides","volume":"29","author":"Lai","year":"2018","journal-title":"J. Am. Soc. Mass Spectrom."},{"issue":"39","key":"2026090306460659300_cit52","doi-asserted-by":"publisher","first-page":"21207","DOI":"10.1021\/jacs.3c08818","article-title":"High Electric\nFields on Water Microdroplets Catalyze Spontaneous\nand Fast Reactions in Halogen-Bond Complexes","volume":"145","author":"Zhu","year":"2023","journal-title":"J. Am. Chem. Soc."}],"container-title":["Analytical Chemistry"],"original-title":[],"language":"en","link":[{"URL":"https:\/\/pubs.acs.org\/doi\/pdf\/10.1021\/acs.analchem.6c02622","content-type":"application\/pdf","content-version":"vor","intended-application":"unspecified"},{"URL":"https:\/\/pubs.acs.org\/ancham\/article-pdf\/98\/34\/25013\/66920390\/acs.analchem.6c02622.pdf","content-type":"application\/pdf","content-version":"vor","intended-application":"syndication"},{"URL":"https:\/\/pubs.acs.org\/ancham\/article-pdf\/98\/34\/25013\/66920390\/acs.analchem.6c02622.pdf","content-type":"unspecified","content-version":"vor","intended-application":"similarity-checking"}],"deposited":{"date-parts":[[2026,9,3]],"date-time":"2026-09-03T10:46:15Z","timestamp":1788432375000},"score":1,"resource":{"primary":{"URL":"https:\/\/pubs.acs.org\/ancham\/article\/98\/34\/25013\/5279320\/Nanoscale-Visualization-of-Microdroplet-Regulated"}},"subtitle":[],"short-title":[],"issued":{"date-parts":[[2026,8,20]]},"references-count":52,"journal-issue":{"issue":"34","published-online":{"date-parts":[[2026,8,20]]},"published-print":{"date-parts":[[2026,9,1]]}},"URL":"https:\/\/doi.org\/10.1021\/acs.analchem.6c02622","relation":{},"ISSN":["0003-2700","1520-6882"],"issn-type":[{"value":"0003-2700","type":"print"},{"value":"1520-6882","type":"electronic"}],"subject":[],"published":{"date-parts":[[2026,8,20]]}}}