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However, catalytic performance is often discussed in terms of active site density alone, while the role of the local interfacial environment remains insufficiently resolved. Here, a series of Printex L6 carbon-supported copper catalysts (PL6C@Cux, where x corresponds to the actual Cu loading wt %) were systematically evaluated for the selective CO2-to-CO conversion. Through linear sweep voltammetry analysis, PL6C@Cu1.04 was identified as the best-performing catalyst among the catalysts investigated; this catalyst exhibited a marked anodic shift in onset potential (to \u22120.53 V vs RHE) compared to the bare PL6C and nonoptimized loadings. Rotating ring-disk electrode measurements confirmed CO as the dominant product, detected via oxidation at \u223c0.8 V vs RHE. To elucidate the mechanistic origins of the enhancement in catalytic efficiency, the interfacial microenvironment was investigated using a quinone redox probe sensitive to local CO2 concentration and adsorption dynamics. The optimized PL6C@Cu1.04 catalyst showed an estimated 15-fold increase in the local CO2 affinity index compared to the bare PL6C catalyst, associated with a 140 mV positive shift in the half-wave potential of the redox probe. This study offers experimental evidence suggesting that optimizing metal loading not only maximizes active sites but also assists in engineering a CO2-enriched microenvironment, which appears crucial for driving efficient and selective electrocatalysis.<\/jats:p>","DOI":"10.1021\/acsomega.6c02410","type":"journal-article","created":{"date-parts":[[2026,8,4]],"date-time":"2026-08-04T22:01:55Z","timestamp":1785880915000},"page":"47626-47637","source":"Crossref","is-referenced-by-count":0,"title":["Interfacial Insights into the Efficient Electroconversion\nof CO2 to CO Using Cu-Based Catalysts Supported on Printex\nL6 Carbon"],"prefix":"10.1021","volume":"11","author":[{"ORCID":"https:\/\/orcid.org\/0000-0003-3018-3322","authenticated-orcid":true,"given":"Thalita F.","family":"da Silva","sequence":"first","affiliation":[{"name":"University of Sa\u0303o Paulo , , Trab. Sa\u0303o Carlense Avenue, 400 , , ,","place":["Sa\u0303o Carlos, Sa\u0303o Paulo, Brazil, 13566-590"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Larissa","family":"T. Cardoso","sequence":"additional","affiliation":[{"name":"University of Sa\u0303o Paulo , , Trab. Sa\u0303o Carlense Avenue, 400 , , ,","place":["Sa\u0303o Carlos, Sa\u0303o Paulo, Brazil, 13566-590"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Marcie\u0301lli K. R.","family":"de Souza","sequence":"additional","affiliation":[{"name":"University of Sa\u0303o Paulo , , Trab. Sa\u0303o Carlense Avenue, 400 , , ,","place":["Sa\u0303o Carlos, Sa\u0303o Paulo, Brazil, 13566-590"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-8654-3844","authenticated-orcid":true,"given":"Julio C.","family":"Lourenc\u0327o","sequence":"additional","affiliation":[{"name":"University of Sa\u0303o Paulo , , Trab. Sa\u0303o Carlense Avenue, 400 , , ,","place":["Sa\u0303o Carlos, Sa\u0303o Paulo, Brazil, 13566-590"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-0768-4156","authenticated-orcid":true,"given":"Guilherme V.","family":"Fortunato","sequence":"additional","affiliation":[{"name":"Technical University Munich , , Campus Straubing, Schulgasse 22 , ,","place":["Straubing, Germany, 94315"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-8285-7838","authenticated-orcid":true,"given":"Marcos R. V.","family":"Lanza","sequence":"additional","affiliation":[{"name":"University of Sa\u0303o Paulo , , Trab. Sa\u0303o Carlense Avenue, 400 , , ,","place":["Sa\u0303o Carlos, Sa\u0303o Paulo, Brazil, 13566-590"]}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"316","published-online":{"date-parts":[[2026,8,4]]},"reference":[{"issue":"16","key":"2026081810495680000_cit1","doi-asserted-by":"publisher","first-page":"2305513","DOI":"10.1002\/smll.202305513","article-title":"Constructing Gold Single-Atom\nCatalysts on Hierarchical Nitrogen-Doped Carbon Nanocages for Carbon\nDioxide Electroreduction to Syngas","volume":"20","author":"Jiao","year":"2024","journal-title":"Small"},{"key":"2026081810495680000_cit2","doi-asserted-by":"publisher","first-page":"119","DOI":"10.1016\/j.jcat.2014.07.001","article-title":"Speciation-Controlled Incipient Wetness\nImpregnation: A Rational Synthetic Approach to Prepare Sub-Nanosized\nand Highly Active Ceria\u2013Zirconia Supported Gold Catalysts","volume":"318","author":"Del Ri\u0301o","year":"2014","journal-title":"J. Catal"},{"issue":"23","key":"2026081810495680000_cit3","doi-asserted-by":"publisher","DOI":"10.1002\/celc.202500170","article-title":"Positioning\nCu in Templated Porous Ag for Active and Selective Electroreduction\nto C2+ Products","volume":"12","author":"Vink-van Ittersum","year":"2025","journal-title":"ChemElectrochem"},{"issue":"1","key":"2026081810495680000_cit4","doi-asserted-by":"publisher","first-page":"5954","DOI":"10.1038\/s41467-020-19369-6","article-title":"A Few Basic\nConcepts in Electrochemical Carbon Dioxide Reduction","volume":"11","author":"Chan","year":"2020","journal-title":"Nat. Commun"},{"issue":"5","key":"2026081810495680000_cit5","doi-asserted-by":"publisher","first-page":"825","DOI":"10.1016\/j.joule.2017.09.003","article-title":"What Should\nWe Make\nwith CO2 and How Can We Make It?","volume":"2","author":"Bushuyev","year":"2018","journal-title":"Joule"},{"issue":"4","key":"2026081810495680000_cit6","doi-asserted-by":"publisher","first-page":"1674","DOI":"10.1002\/anie.201912637","article-title":"Direct Evidence of Local PH Change\nand the Role of Alkali Cation\nduring CO2 Electroreduction in Aqueous Media","volume":"59","author":"Zhang","year":"2020","journal-title":"Angew. Chem., Int. Ed"},{"key":"2026081810495680000_cit7","doi-asserted-by":"publisher","first-page":"151849","DOI":"10.1016\/j.cej.2024.151849","article-title":"Surface-Modified Silver Aerogels Combining Interfacial\nRegulation\nfor Electrocatalytic CO2 Reduction under Large Current\nDensity","volume":"490","author":"Wang","year":"2024","journal-title":"Chem. Eng. J"},{"key":"2026081810495680000_cit8","doi-asserted-by":"publisher","first-page":"160286","DOI":"10.1016\/j.cej.2025.160286","article-title":"Paired Electrolysis\nfor Efficient Coproduction of CO and S8 with Techno-Economic\nAnalysis","volume":"507","author":"Gong","year":"2025","journal-title":"Chem. Eng.\nJ"},{"issue":"1","key":"2026081810495680000_cit9","doi-asserted-by":"publisher","first-page":"8704","DOI":"10.1038\/s41467-025-63722-6","article-title":"Interface Engineering\nof Single-Molecular Heterojunction\nCatalysts for CO2 Electroreduction in Strong Acid Medium","volume":"16","author":"Gong","year":"2025","journal-title":"Nat. Commun"},{"issue":"14","key":"2026081810495680000_cit10","doi-asserted-by":"publisher","DOI":"10.1002\/smll.202514230","article-title":"Promoting\nElectrocatalytic CO2 Reduction via Oxophilic Amorphous\nMetal Oxide-Mediated Interfacial\nWater Activation and Structure Evolution","volume":"22","author":"Wang","year":"2026","journal-title":"Small"},{"key":"2026081810495680000_cit11","doi-asserted-by":"publisher","first-page":"89","DOI":"10.1007\/978-0-387-49489-0_3","article-title":"Electrochemical\nCO2 Reduction on Metal Electrodes","volume-title":"Modern Aspects of Electrochemistry","author":"Hori","year":"2008"},{"issue":"12","key":"2026081810495680000_cit12","doi-asserted-by":"publisher","first-page":"8461","DOI":"10.1021\/acs.nanolett.9b02748","article-title":"Copper Nanocubes for CO2 Reduction in Gas Diffusion Electrodes","volume":"19","author":"Wang","year":"2019","journal-title":"Nano\nLett"},{"issue":"7620","key":"2026081810495680000_cit13","doi-asserted-by":"publisher","first-page":"382","DOI":"10.1038\/nature19060","article-title":"Enhanced Electrocatalytic CO2 Reduction\nvia Field-Induced Reagent Concentration","volume":"537","author":"Liu","year":"2016","journal-title":"Nature"},{"issue":"9","key":"2026081810495680000_cit14","doi-asserted-by":"publisher","first-page":"104108","DOI":"10.1016\/j.apt.2023.104108","article-title":"Using ZrNb and ZrMo Oxide Nanoparticles\nas Catalytic Activity Boosters Supported on Printex L6 Carbon for\nH2O2 Production","volume":"34","author":"Trevelin","year":"2023","journal-title":"Adv.\nPowder Technol"},{"key":"2026081810495680000_cit15","doi-asserted-by":"publisher","first-page":"164432","DOI":"10.1016\/j.cej.2025.164432","article-title":"In-Situ\nElectrogeneration of H2O2 and Hydroxyl Radical\nApplied for Venlafaxine Degradation: A Novel Strategy Using FeSe2-Modified Carbon Gas Diffusion Electrode","volume":"517","author":"Bimbi Ju\u0301nior","year":"2025","journal-title":"Chem. Eng. J"},{"issue":"1","key":"2026081810495680000_cit16","doi-asserted-by":"publisher","first-page":"1956","DOI":"10.1038\/s41467-025-57307-6","article-title":"Electronic Metal-Support\nInteraction Modulates Cu Electronic Structures for CO2 Electroreduction\nto Desired Products","volume":"16","author":"Zhang","year":"2025","journal-title":"Nat. Commun"},{"key":"2026081810495680000_cit17","doi-asserted-by":"publisher","first-page":"169","DOI":"10.1016\/j.jechem.2023.09.005","article-title":"Single Atom Cu-N-C Catalysts for\nthe Electro-Reduction of CO2 to CO Assessed by Rotating\nRing-Disc Electrode","volume":"88","author":"Pe\u0301rez-Rodri\u0301guez","year":"2024","journal-title":"J. Energy Chem"},{"issue":"4","key":"2026081810495680000_cit18","doi-asserted-by":"publisher","first-page":"046517","DOI":"10.1149\/1945-7111\/ab7a80","article-title":"Rapid Product Analysis\nfor the Electroreduction of CO2 on Heterogeneous and Homogeneous\nCatalysts Using a Rotating Ring\nDetector","volume":"167","author":"Zhang","year":"2020","journal-title":"J. Electrochem. Soc"},{"issue":"9","key":"2026081810495680000_cit19","doi-asserted-by":"publisher","first-page":"4154","DOI":"10.1021\/jacs.9b10061","article-title":"Competition between\nCO2 Reduction and Hydrogen Evolution on a Gold Electrode\nunder Well-Defined Mass Transport Conditions","volume":"142","author":"Goyal","year":"2020","journal-title":"J. Am. Chem. Soc"},{"issue":"11","key":"2026081810495680000_cit20","doi-asserted-by":"publisher","first-page":"3288","DOI":"10.1039\/D1SC05743J","article-title":"Effect of Pore\nDiameter and Length on Electrochemical CO2 Reduction Reaction\nat Nanoporous Gold Catalysts","volume":"13","author":"Goyal","year":"2022","journal-title":"Chem. Sci"},{"issue":"34","key":"2026081810495680000_cit21","doi-asserted-by":"publisher","first-page":"17691","DOI":"10.1039\/D0TA05908K","article-title":"Developing\nEfficient Catalysts for the OER and ORR Using a Combination\nof Co, Ni, and Pt Oxides along with Graphene Nanoribbons and NiCo2O4","volume":"8","author":"Bezerra","year":"2020","journal-title":"J. Mater. Chem. A"},{"issue":"21","key":"2026081810495680000_cit22","doi-asserted-by":"publisher","first-page":"6224","DOI":"10.1039\/D4CY00781F","article-title":"New Insights into Influences of Initial Oxidization\nStates on Dynamic Reconstruction of Cu Catalysts and C\u2013C Coupling\nin CO2 Reduction","volume":"14","author":"Qin","year":"2024","journal-title":"Catal. Sci. Technol"},{"key":"2026081810495680000_cit23","doi-asserted-by":"publisher","first-page":"1","DOI":"10.1155\/2018\/9875438","article-title":"Spiky Nickel\nElectrodes for Electrochemical Oxygen Evolution Catalysis by Femtosecond\nLaser Structuring","volume":"2018","author":"Rieck Genannt Best","year":"2018","journal-title":"Int. J. Electrochem"},{"issue":"45","key":"2026081810495680000_cit24","doi-asserted-by":"publisher","first-page":"16977","DOI":"10.1021\/ja407115p","article-title":"Benchmarking\nHeterogeneous Electrocatalysts for the Oxygen Evolution Reaction","volume":"135","author":"McCrory","year":"2013","journal-title":"J. Am. Chem. Soc"},{"key":"2026081810495680000_cit25","doi-asserted-by":"publisher","first-page":"1009","DOI":"10.1016\/j.ijhydene.2025.02.246","article-title":"Electrocatalysts\nfor Hydrogen and Oxygen Evolution\nReactions under Neutral\/near-Neutral Conditions: Summary and Challenges","volume":"137","author":"Irshad","year":"2025","journal-title":"Int. J. Hydrogen Energy"},{"issue":"3","key":"2026081810495680000_cit26","doi-asserted-by":"publisher","first-page":"278","DOI":"10.1021\/acsmaterialsau.1c00067","article-title":"Electrochemical\nSurface Area Quantification, CO2 Reduction Performance,\nand Stability Studies of Unsupported Three-Dimensional Au Aerogels\nversus Carbon-Supported Au Nanoparticles","volume":"2","author":"Chauhan","year":"2022","journal-title":"ACS\nMater. Au"},{"issue":"431","key":"2026081810495680000_cit27","doi-asserted-by":"publisher","first-page":"114579","DOI":"10.1016\/j.cattod.2024.114579","article-title":"Development of a TiO2 Nanotube Photoanode\nDecorated with MIL-53(Fe) for the Photoelectrochemical Degradation\nof 2,4-Dimethylaniline","volume":"431","author":"da Silva","year":"2024","journal-title":"Catal. Today"},{"key":"2026081810495680000_cit28","doi-asserted-by":"publisher","first-page":"1037","DOI":"10.1016\/j.electacta.2018.07.025","article-title":"Electrochemical\nReduction of Carbon Dioxide on Copper-Based\nNanocatalysts Using the Rotating Ring-Disc Electrode","volume":"283","author":"Zhu","year":"2018","journal-title":"Electrochim. Acta"},{"issue":"47","key":"2026081810495680000_cit29","doi-asserted-by":"publisher","first-page":"26785","DOI":"10.1039\/C9TA10111J","article-title":"The Sensitivity of\nCu for Electrochemical Carbon Dioxide\nReduction to Hydrocarbons as Revealed by High Throughput Experiments","volume":"7","author":"Lai","year":"2019","journal-title":"J. Mater. Chem. A"},{"key":"2026081810495680000_cit30","doi-asserted-by":"publisher","first-page":"121847","DOI":"10.1016\/j.seppur.2022.121847","article-title":"Electrochemical Production of Extremely\nHigh Concentrations of Hydrogen Peroxide in Discontinuous Processes","volume":"300","author":"Marques Cordeiro-Junior","year":"2022","journal-title":"Sep. Purif. Technol"},{"issue":"19","key":"2026081810495680000_cit31","doi-asserted-by":"publisher","first-page":"6978","DOI":"10.1021\/ja500328k","article-title":"Particle Size Effects in the Catalytic Electroreduction\nof CO2 on Cu Nanoparticles","volume":"136","author":"Reske","year":"2014","journal-title":"J. Am.\nChem. Soc"},{"issue":"27","key":"2026081810495680000_cit32","doi-asserted-by":"publisher","first-page":"13872","DOI":"10.1021\/jp403655y","article-title":"Structure-Dependent Electrocatalytic Properties of\nCu2O Nanocrystals for Oxygen Reduction Reaction","volume":"117","author":"Li","year":"2013","journal-title":"J. Phys. Chem. C"},{"issue":"13","key":"2026081810495680000_cit33","doi-asserted-by":"publisher","first-page":"9557","DOI":"10.1021\/acs.energyfuels.3c00452","article-title":"Electronic Modulation\nof Pd\/C by Simultaneous Doping\nof Cu and Co Tendering a Highly Durable and Methanol-Tolerant Oxygen\nReduction Electrocatalyst","volume":"37","author":"Chetry","year":"2023","journal-title":"Energy Fuels"},{"issue":"8","key":"2026081810495680000_cit34","doi-asserted-by":"publisher","first-page":"2842","DOI":"10.1016\/j.carbon.2011.03.014","article-title":"A Comparative Study\nof the Electrogeneration of Hydrogen Peroxide Using Vulcan and Printex\nCarbon Supports","volume":"49","author":"Assumpc\u0327a\u0303o","year":"2011","journal-title":"Carbon"},{"key":"2026081810495680000_cit35","doi-asserted-by":"publisher","DOI":"10.1002\/adfm.202514183","article-title":"Highly Selective Toward HER or CO2RR by Regulating Cu\nSingle and Dual Atoms on G-C3N4","volume":"36","author":"Chen","year":"2026","journal-title":"Adv. Funct. Mater"},{"key":"2026081810495680000_cit36","doi-asserted-by":"publisher","first-page":"56","DOI":"10.1016\/j.jcat.2020.09.020","article-title":"Catalysis of Oxygen Reduction Reaction\nfor H2O2 Electrogeneration: The Impact of Different\nConductive Carbon Matrices and Their Physicochemical Properties","volume":"392","author":"Cordeiro-Junior","year":"2020","journal-title":"J. Catal"},{"issue":"2","key":"2026081810495680000_cit37","doi-asserted-by":"publisher","first-page":"12","DOI":"10.1007\/s40828-020-0110-7","article-title":"A Tutorial on Electrochemical Impedance\nSpectroscopy","volume":"6","author":"Orazem","year":"2020","journal-title":"ChemTexts"},{"issue":"2","key":"2026081810495680000_cit38","doi-asserted-by":"publisher","first-page":"161","DOI":"10.1007\/s10800-005-9058-y","article-title":"Calculation\nfor the Cathode Surface\nConcentrations in the Electrochemical Reduction of CO2 in\nKHCO3 Solutions","volume":"36","author":"Gupta","year":"2006","journal-title":"J. Appl. Electrochem"},{"issue":"1","key":"2026081810495680000_cit39","doi-asserted-by":"publisher","first-page":"5843","DOI":"10.1038\/s41467-022-33589-y","article-title":"Volcano-Type\nRelationship between Oxidation States and Catalytic Activity of Single-Atom\nCatalysts towards Hydrogen Evolution","volume":"13","author":"Cao","year":"2022","journal-title":"Nat. Commun"},{"issue":"7","key":"2026081810495680000_cit40","doi-asserted-by":"publisher","first-page":"076503","DOI":"10.1149\/1945-7111\/ad5da0","article-title":"Electrochemical CO2 Reduction at Surface Modified Silver\nNanoparticles","volume":"171","author":"Trevino","year":"2024","journal-title":"J. Electrochem. Soc"},{"issue":"14","key":"2026081810495680000_cit41","doi-asserted-by":"publisher","first-page":"1900","DOI":"10.1021\/acs.accounts.2c00080","article-title":"Electrolyte Effects\non CO2 Electrochemical Reduction to CO","volume":"55","author":"Marcandalli","year":"2022","journal-title":"Acc. Chem. Res"},{"issue":"22","key":"2026081810495680000_cit42","doi-asserted-by":"publisher","first-page":"9708","DOI":"10.1021\/acs.jpclett.0c02779","article-title":"Understanding\nthe Voltammetry of\nBulk CO Electrooxidation in Neutral Media through Combined SECM Measurements","volume":"11","author":"Monteiro","year":"2020","journal-title":"J. Phys. Chem. Lett"},{"issue":"12","key":"2026081810495680000_cit43","doi-asserted-by":"publisher","first-page":"4398","DOI":"10.1021\/acsenergylett.2c02021","article-title":"Interfacial\nO2 Accumulation Affects Microenvironment in Carbon-Based\nElectrocatalysts for H2O2 Production","volume":"7","author":"Yang","year":"2022","journal-title":"ACS Energy Lett"},{"issue":"10","key":"2026081810495680000_cit44","doi-asserted-by":"publisher","first-page":"1194","DOI":"10.1134\/S1023193517100135","article-title":"Rotating Ring-Disk Voltammetry: Diagnosis of Catalytic\nActivity of Metallic Copper Catalysts toward CO2 Electroreduction","volume":"53","author":"Wadas","year":"2017","journal-title":"Russ. J. Electrochem"},{"issue":"9","key":"2026081810495680000_cit45","doi-asserted-by":"publisher","first-page":"1878","DOI":"10.1021\/acselectrochem.5c00295","article-title":"Determining\nthe Faradaic Efficiency\nand Selectivity Using a Rotating Ring-Disk Electrode at Low and Intermediate\nRotation Rates: Example of the Oxygen Reduction Reaction on Carbon\nMaterials","volume":"1","author":"Olean-Oliveira","year":"2025","journal-title":"ACS Electrochem"},{"issue":"3","key":"2026081810495680000_cit46","doi-asserted-by":"publisher","first-page":"2015","DOI":"10.1021\/jacs.3c10610","article-title":"Gold Nanoparticles for CO2 Electroreduction: An Optimum Defined by Size and Shape","volume":"146","author":"Sedano Varo","year":"2024","journal-title":"J. Am. Chem. 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