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Directly resolving this interplay under reaction conditions remains challenging because it requires simultaneous chemical sensitivity and nanoscale spatial resolution. Here, we employ in situ electrochemical tip-enhanced Raman spectroscopy (EC-TERS) to track CO electrooxidation on individual Pd nanocatalysts with sub-30 nm dimensions at a spatial resolution of 3 nm. Hyperspectral imaging reveals that oxidation is initiated at low-coordinated edge sites, manifested as preferential CO depletion at the particle periphery. At the same time, a continuous red shift of the C\u2013O stretching mode on terrace sites indicates a decrease in the local CO coverage. Together with the preferential CO depletion at edge sites, this spatial and spectral evolution reveals terrace-to-edge CO migration during electrooxidation. These observations suggest that surface migration contributes to sustaining the reaction and may play a rate-limiting role during the early stages of electrooxidation. Across Pd nanocatalysts with different local structures, the migration behavior evolves differently, linking the nanoscale structure to electrocatalytic performance. More broadly, this work demonstrates how spatially resolved chemical imaging can disentangle site-specific reactivity and molecular migration, providing a framework for understanding migration-mediated electrocatalysis at complex electrochemical interfaces.<\/jats:p>","DOI":"10.1021\/jacs.6c14102","type":"journal-article","created":{"date-parts":[[2026,10,8]],"date-time":"2026-10-08T18:02:25Z","timestamp":1791482545000},"page":"44748-44756","source":"Crossref","is-referenced-by-count":0,"title":["Visualizing the Site-Specific\nKinetics and Terrace-to-Edge\nMigration of CO Electrooxidation on a Single Pd Nanocatalyst"],"prefix":"10.1021","volume":"148","author":[{"ORCID":"https:\/\/orcid.org\/0009-0007-3962-0361","authenticated-orcid":true,"given":"Yi-Fan","family":"Bao","sequence":"first","affiliation":[{"name":"Xiamen University , , ,","place":["Xiamen, China, 361005"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Meng-Yuan","family":"Zhu","sequence":"additional","affiliation":[{"name":"Xiamen University , , ,","place":["Xiamen, China, 361005"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-8341-4003","authenticated-orcid":true,"given":"Hao","family":"Ma","sequence":"additional","affiliation":[{"name":"Xiamen University , , ,","place":["Xiamen, China, 361005"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Hong-Xuan","family":"Chen","sequence":"additional","affiliation":[{"name":"Xiamen University , , ,","place":["Xiamen, China, 361005"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Nan-Nan","family":"Zhang","sequence":"additional","affiliation":[{"name":"Xiamen University , , ,","place":["Xiamen, China, 361005"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Jia-Yi","family":"Wang","sequence":"additional","affiliation":[{"name":"Xiamen University , , ,","place":["Xiamen, China, 361005"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Xin-Yu","family":"Lu","sequence":"additional","affiliation":[{"name":"Xiamen University , , ,","place":["Xiamen, China, 361005"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-2501-7178","authenticated-orcid":true,"given":"Guo-Kun","family":"Liu","sequence":"additional","affiliation":[{"name":"Xiamen University , , ,","place":["Xiamen, China, 361005"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-1937-0725","authenticated-orcid":true,"given":"Xiang","family":"Wang","sequence":"additional","affiliation":[{"name":"Xiamen University , , ,","place":["Xiamen, China, 361005"]},{"name":"Innovation Laboratory for Sciences and Technologies of Energy Materials of Fujian Province (IKKEM) , ,","place":["Xiamen, China, 361005"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-9821-5864","authenticated-orcid":true,"given":"Bin","family":"Ren","sequence":"additional","affiliation":[{"name":"Xiamen University , , ,","place":["Xiamen, China, 361005"]},{"name":"Innovation Laboratory for Sciences and Technologies of Energy Materials of Fujian Province (IKKEM) , ,","place":["Xiamen, China, 361005"]}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"316","published-online":{"date-parts":[[2026,10,8]]},"reference":[{"key":"2026102111080847200_cit1","doi-asserted-by":"publisher","DOI":"10.1038\/s41570-016-0003","article-title":"Earth-abundant catalysts for electrochemical\nand photoelectrochemical water splitting","volume":"1","author":"Roger","year":"2017","journal-title":"Nat.\nRev. 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Rev."},{"key":"2026102111080847200_cit5","doi-asserted-by":"publisher","first-page":"105","DOI":"10.1098\/rspa.1925.0061","article-title":"A theory\nof the catalytic surface","volume":"108","author":"Taylor","year":"1925","journal-title":"Proc. R. Soc. London,\nSer. A"},{"key":"2026102111080847200_cit6","doi-asserted-by":"publisher","first-page":"539","DOI":"10.1016\/S0009-2614(97)00916-0","article-title":"Effect\nof molecular mobility on kinetics of an electrochemical Langmuir-Hinshelwood\nreaction","volume":"277","author":"Petukhov","year":"1997","journal-title":"Chem. Phys. Lett."},{"key":"2026102111080847200_cit7","doi-asserted-by":"publisher","first-page":"885","DOI":"10.1038\/s41929-023-01002-6","article-title":"Experimental evidence\nof distinct sites for CO2-to-CO and CO conversion on Cu\nin the electrochemical CO2 reduction reaction","volume":"6","author":"Gao","year":"2023","journal-title":"Nat. Catal."},{"key":"2026102111080847200_cit8","doi-asserted-by":"publisher","first-page":"74","DOI":"10.1038\/nature23661","article-title":"Direct\ninstrumental identification of catalytically active surface sites","volume":"549","author":"Pfisterer","year":"2017","journal-title":"Nature"},{"key":"2026102111080847200_cit9","doi-asserted-by":"publisher","first-page":"11618","DOI":"10.1073\/pnas.1821091116","article-title":"Direct high-resolution\nmapping of electrocatalytic activity of semi-two-dimensional catalysts\nwith single-edge sensitivity","volume":"116","author":"Sun","year":"2019","journal-title":"Proc. Natl. Acad.\nSci. U.S.A."},{"key":"2026102111080847200_cit10","doi-asserted-by":"publisher","first-page":"67","DOI":"10.1038\/s41586-021-03454-x","article-title":"Correlative operando microscopy of oxygen evolution\nelectrocatalysts","volume":"593","author":"Mefford","year":"2021","journal-title":"Nature"},{"key":"2026102111080847200_cit11","doi-asserted-by":"publisher","first-page":"242","DOI":"10.1016\/S0022-0728(02)00669-1","article-title":"Mechanism\nand kinetics of the electrochemical CO adlayer oxidation on Pt(111)","volume":"524\u2013525","author":"Lebedeva","year":"2002","journal-title":"J. Electroanal. 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Electrochem."},{"key":"2026102111080847200_cit18","doi-asserted-by":"publisher","DOI":"10.1038\/s43586-023-00263-6","article-title":"Electrochemical surface-enhanced Raman spectroscopy","volume":"3","author":"Brosseau","year":"2023","journal-title":"Nat. Rev. Methods Primers"},{"key":"2026102111080847200_cit19","doi-asserted-by":"publisher","first-page":"14000","DOI":"10.1021\/acsnano.4c02670","article-title":"Surface-Enhanced\nRaman Spectroscopy: Current Understanding, Challenges, and Opportunities","volume":"18","author":"Ma","year":"2024","journal-title":"ACS Nano"},{"key":"2026102111080847200_cit20","first-page":"357","article-title":"Surfaced-Enhanced\nRaman Spectroscopy (SERS) 50 Years: Theories, Applications and Perspectives","volume":"37","author":"Ma","year":"2025","journal-title":"Chin. J. Light Scatter."},{"key":"2026102111080847200_cit21","doi-asserted-by":"publisher","first-page":"3579","DOI":"10.1039\/D3CS00734K","article-title":"Sixty years\nof electrochemical optical spectroscopy:\na retrospective","volume":"53","author":"Li","year":"2024","journal-title":"Chem. Soc. Rev."},{"key":"2026102111080847200_cit22","doi-asserted-by":"publisher","first-page":"11928","DOI":"10.1021\/jacs.5b08143","article-title":"Electrochemical Tip-Enhanced\nRaman Spectroscopy","volume":"137","author":"Zeng","year":"2015","journal-title":"J. Am. Chem. Soc."},{"key":"2026102111080847200_cit23","doi-asserted-by":"publisher","first-page":"7956","DOI":"10.1021\/acs.nanolett.5b04177","article-title":"Probing\nRedox Reactions at the Nanoscale\nwith Electrochemical Tip-Enhanced Raman Spectroscopy","volume":"15","author":"Kurouski","year":"2015","journal-title":"Nano Lett."},{"key":"2026102111080847200_cit24","doi-asserted-by":"publisher","DOI":"10.1016\/j.surfrep.2026.100686","article-title":"Electrochemical\ntip-enhanced Raman spectroscopy: a decade of nanoscale insights into\nthe electrochemical interface","volume":"81","author":"Zhu","year":"2026","journal-title":"Surf. Sci. Rep."},{"key":"2026102111080847200_cit25","doi-asserted-by":"publisher","first-page":"2791","DOI":"10.1021\/acs.analchem.3c02601","article-title":"Electrochemical\nTip-Enhanced Raman\nSpectroscopy for the Elucidation of Complex Electrochemical Reactions","volume":"96","author":"Fiocco","year":"2024","journal-title":"Anal. Chem."},{"key":"2026102111080847200_cit26","doi-asserted-by":"publisher","first-page":"12568","DOI":"10.1021\/acs.jpcc.3c01828","article-title":"Probing the Intermediate\nin the Electrochemical\nReduction of Nitrobenzene Derivative by EC-TERS","volume":"127","author":"Huang","year":"2023","journal-title":"J. Phys. Chem. C"},{"key":"2026102111080847200_cit27","doi-asserted-by":"publisher","first-page":"15684","DOI":"10.1021\/jacs.9b07979","article-title":"Operando Characterization of Iron\nPhthalocyanine Deactivation\nduring Oxygen Reduction Reaction Using Electrochemical Tip-Enhanced\nRaman Spectroscopy","volume":"141","author":"Chen","year":"2019","journal-title":"J. Am. Chem. Soc."},{"key":"2026102111080847200_cit28","doi-asserted-by":"publisher","DOI":"10.1038\/s41467-019-13692-3","article-title":"Reactivity mapping\nof nanoscale defect chemistry under electrochemical reaction conditions","volume":"10","author":"Pfisterer","year":"2019","journal-title":"Nat. Commun."},{"key":"2026102111080847200_cit29","doi-asserted-by":"publisher","first-page":"646","DOI":"10.1038\/s41929-024-01148-x","article-title":"Visualizing\nthe structural evolution\nof individual active sites in MoS2 during electrocatalytic\nhydrogen evolution reaction","volume":"7","author":"Huang","year":"2024","journal-title":"Nat. Catal."},{"key":"2026102111080847200_cit30","doi-asserted-by":"publisher","first-page":"753","DOI":"10.1038\/s41929-025-01395-6","article-title":"The critical role of\nlocal microenvironments","volume":"8","author":"Geng","year":"2025","journal-title":"Nat. Catal."},{"key":"2026102111080847200_cit31","doi-asserted-by":"publisher","first-page":"117","DOI":"10.1016\/S0167-5729(01)00022-X","article-title":"Surface science studies of model\nfuel cell electrocatalysts","volume":"45","author":"Markovic\u0301","year":"2002","journal-title":"Surf. Sci. Rep."},{"key":"2026102111080847200_cit32","doi-asserted-by":"publisher","first-page":"70","DOI":"10.1021\/j100783a013","article-title":"The mechanism\nof electrochemical oxidation of carbon monoxide and methanol on platinum.\nII. The \u201cReactant-Pair\u201d mechanism for electrochemical\noxidation of carbon monoxide and Methanol","volume":"68","author":"Gilman","year":"1964","journal-title":"J.\nPhys. Chem. A"},{"key":"2026102111080847200_cit33","doi-asserted-by":"publisher","first-page":"6051","DOI":"10.1063\/1.477230","article-title":"Monte\nCarlo simulations of a simple model for the electrocatalytic CO oxidation\non platinum","volume":"109","author":"Koper","year":"1998","journal-title":"J. Chem. Phys."},{"key":"2026102111080847200_cit34","doi-asserted-by":"publisher","first-page":"277","DOI":"10.1016\/S0022-0728(76)80196-9","article-title":"An investigation of\nthe mechanism of the oxidation\nof carbon monoxide adsorbed onto a smooth Pt electrode in aqueous\nacid","volume":"70","author":"McCallum","year":"1976","journal-title":"J. Electroanal. Chem. Interfacial Electrochem."},{"key":"2026102111080847200_cit35","doi-asserted-by":"publisher","first-page":"155","DOI":"10.1016\/S0022-0728(99)00329-0","article-title":"Infrared spectroscopy of carbon monoxide\nand nitric oxide on palladium(111) in aqueous solution: unexpected\nadlayer structural differences between electrochemical and ultrahigh-vacuum\ninterfaces","volume":"474","author":"Zou","year":"1999","journal-title":"J. Electroanal. Chem."},{"key":"2026102111080847200_cit36","doi-asserted-by":"publisher","first-page":"10222","DOI":"10.1021\/jp900582c","article-title":"Dynamics of\nCO Oxidation on a Polycrystalline\nPlatinum Electrode: A Time-Resolved Infrared Study","volume":"113","author":"Samjeske\u0301","year":"2009","journal-title":"J. Phys. Chem. C"},{"key":"2026102111080847200_cit37","doi-asserted-by":"publisher","first-page":"16378","DOI":"10.1021\/jp104181y","article-title":"Study of CO Oxidation\non Polycrystalline Pt Electrodes in Acidic Solution by ATR-SEIRAS","volume":"115","author":"Yan","year":"2011","journal-title":"J. Phys. Chem. C"},{"key":"2026102111080847200_cit38","doi-asserted-by":"publisher","first-page":"121","DOI":"10.1016\/j.jelechem.2007.02.020","article-title":"Active site model for CO adlayer electrooxidation on\nnanoparticle catalysts","volume":"607","author":"Andreaus","year":"2007","journal-title":"J. Electroanal. Chem."},{"key":"2026102111080847200_cit39","doi-asserted-by":"publisher","first-page":"12938","DOI":"10.1021\/jp0204105","article-title":"Role of\nCrystalline Defects in Electrocatalysis: Mechanism and Kinetics of\nCO Adlayer Oxidation on Stepped Platinum Electrodes","volume":"106","author":"Lebedeva","year":"2002","journal-title":"J. Phys. Chem. B"},{"key":"2026102111080847200_cit40","doi-asserted-by":"publisher","first-page":"16109","DOI":"10.1021\/acs.analchem.4c02267","article-title":"Micro Reference Electrode with an Ultrathin Ionic Path","volume":"96","author":"Zhu","year":"2024","journal-title":"Anal. Chem."},{"key":"2026102111080847200_cit41","doi-asserted-by":"publisher","first-page":"9149","DOI":"10.1021\/acsami.5c21414","article-title":"Facile Electrochemical\nTwo-Step Etching to Improve\nthe Performance of Au Tips in Tip-Enhanced Raman Spectroscopy","volume":"18","author":"Chen","year":"2026","journal-title":"ACS Appl. Mater. Interfaces"},{"key":"2026102111080847200_cit42","doi-asserted-by":"publisher","first-page":"5953","DOI":"10.1021\/ac0106391","article-title":"Surface-Enhanced\nRaman Scattering on Uniform Platinum-Group\nOverlayers: Preparation by Redox Replacement of Underpotential-Deposited\nMetals on Gold","volume":"73","author":"Mrozek","year":"2001","journal-title":"Anal. Chem."},{"key":"2026102111080847200_cit43","doi-asserted-by":"publisher","first-page":"1105","DOI":"10.1021\/jp0652906","article-title":"Palladium-Coated\nGold Nanoparticles with a Controlled\nShell Thickness Used as Surface-Enhanced Raman Scattering Substrate","volume":"111","author":"Hu","year":"2007","journal-title":"J. Phys. Chem. C"},{"key":"2026102111080847200_cit44","doi-asserted-by":"publisher","first-page":"79","DOI":"10.1016\/j.jelechem.2005.10.016","article-title":"Infrared reflection\nabsorption spectroscopy of carbon monoxide adsorbed on Pd(S)-[n(111)\u00d7(111)]\nand Pd(S)-[n(100)\u00d7(111)] electrodes","volume":"587","author":"Hoshi","year":"2006","journal-title":"J.\nElectroanal. Chem."},{"key":"2026102111080847200_cit45","doi-asserted-by":"publisher","first-page":"1177","DOI":"10.1134\/S1023193506110048","article-title":"Electrocatalytic\nproperties of Au(111)-Pd\nquasi-single-crystal film electrodes as probed by ATR-SEIRAS","volume":"42","author":"Pronkin","year":"2006","journal-title":"Russ. J. Electrochem."},{"key":"2026102111080847200_cit46","doi-asserted-by":"publisher","first-page":"9863","DOI":"10.1021\/jp0203806","article-title":"Role of Crystalline Defects in Electrocatalysis: CO\nAdsorption and Oxidation on Stepped Platinum Electrodes As Studied\nby in situ Infrared Spectroscopy","volume":"106","author":"Lebedeva","year":"2002","journal-title":"J. Phys. Chem.\nB"},{"key":"2026102111080847200_cit47","doi-asserted-by":"publisher","DOI":"10.1103\/PhysRevLett.87.056103","article-title":"Oxygen Dissociation\nat Pt Steps","volume":"87","author":"Gambardella","year":"2001","journal-title":"Phys. Rev. Lett."},{"key":"2026102111080847200_cit48","doi-asserted-by":"publisher","first-page":"5603","DOI":"10.1021\/la980495u","article-title":"Nanoscale Island\nFormation during Oxidation of Carbon\nMonoxide Adlayers at Ordered Electrochemical Interfaces: A Dipole-Coupling\nAnalysis of Coverage-Dependent Infrared Spectra","volume":"14","author":"Severson","year":"1998","journal-title":"Langmuir"},{"key":"2026102111080847200_cit49","doi-asserted-by":"publisher","first-page":"2931","DOI":"10.1021\/la9817720","article-title":"Coverage-Dependent Infrared Spectroscopy\nof Carbon Monoxide on Palladium(100) in Aqueous Solution: Adlayer\nPhase Transitions and Electrooxidation Pathways","volume":"15","author":"Zou","year":"1999","journal-title":"Langmuir"},{"key":"2026102111080847200_cit50","doi-asserted-by":"publisher","first-page":"4582","DOI":"10.1063\/1.457719","article-title":"Coverage-dependent\ndipole coupling for carbon monoxide\nadsorbed at ordered platinum(111)-aqueous interfaces: Structural and\nelectrochemical implications","volume":"92","author":"Chang","year":"1990","journal-title":"J. Chem. Phys."},{"key":"2026102111080847200_cit51","doi-asserted-by":"publisher","first-page":"4237","DOI":"10.1021\/jp9533178","article-title":"Potential-Dependent\nMetal-Adsorbate Stretching Frequencies\nfor Carbon Monoxide on Transition-Metal Electrodes: Chemical Bonding\nversus Electrostatic Field Effects","volume":"100","author":"Zou","year":"1996","journal-title":"J. Phys.\nChem. A"},{"key":"2026102111080847200_cit52","doi-asserted-by":"publisher","first-page":"623","DOI":"10.1016\/0013-4686(95)00349-5","article-title":"Vibrational\nStark effect of adsorbates at electrochemical interfaces","volume":"41","author":"Lambert","year":"1996","journal-title":"Electrochim. 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Chem.\nPhys."},{"key":"2026102111080847200_cit55","doi-asserted-by":"publisher","first-page":"11040","DOI":"10.1021\/jp301292p","article-title":"New Insights\ninto the Mechanism and Kinetics of Adsorbed CO Electrooxidation on\nPlatinum: Online Mass Spectrometry and Kinetic Monte Carlo Simulation\nStudies","volume":"116","author":"Wang","year":"2012","journal-title":"J. Phys. Chem. 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