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Direct probing of nanoscale charge dynamics remains limited by the lack of efficient operando techniques. Herein, we develop an electrochemical pump\u2013probe spectroscopy platform to track transient nano-interfacial processes in real time. Featuring high spectral sensitivity and microsecond-to-millisecond resolution, this setup synchronously captures electrical and plasmonic signals to resolve charge relaxation and EDL dynamics of Au nanoparticle electrodes during hydrogen evolution. Correlated electrical and optical responses successfully decouple charge transport and accumulation in electrode and interfacial charge transfer on the electrode surface: the former is more closed to capacitive charging, while the latter is determined by ion diffusion. Such interfacial kinetics are precisely modulated by electrolyte concentration, applied bias, and cation hydration. This work elucidates intrinsic nanoscale EDL evolution under hydrogen evolution reaction (HER) conditions and provides a versatile operando tool for broad nanoelectrochemical studies.<\/jats:p>","DOI":"10.1021\/acs.nanolett.6c03374","type":"journal-article","created":{"date-parts":[[2026,9,21]],"date-time":"2026-09-21T15:02:13Z","timestamp":1790002933000},"page":"13019-13026","source":"Crossref","is-referenced-by-count":0,"title":["Operando Electrochemical\nPump\u2013Probe Spectroscopy\nfor Resolving Electric Double Layer Formation Kinetics at Hydrogen\nEvolution Electrodes"],"prefix":"10.1021","volume":"26","author":[{"given":"Jiping","family":"Sui","sequence":"first","affiliation":[{"name":"Jilin University , , ,","place":["Changchun, China, 130012"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Dangzheng","family":"Hu","sequence":"additional","affiliation":[{"name":"Jilin University , , ,","place":["Changchun, China, 130012"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Meng","family":"Li","sequence":"additional","affiliation":[{"name":"Jilin University , , ,","place":["Changchun, China, 130012"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-0083-6804","authenticated-orcid":true,"given":"Nan","family":"Lin","sequence":"additional","affiliation":[{"name":"Jilin University , , ,","place":["Changchun, China, 130012"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Haibo","family":"Lin","sequence":"additional","affiliation":[{"name":"Jilin University , , ,","place":["Changchun, China, 130012"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Bing","family":"Zhao","sequence":"additional","affiliation":[{"name":"Jilin University , , ,","place":["Changchun, China, 130012"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-4392-7995","authenticated-orcid":true,"given":"Yinghui","family":"Wang","sequence":"additional","affiliation":[{"name":"Jilin University , , ,","place":["Changchun, China, 130012"]}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"316","published-online":{"date-parts":[[2026,9,21]]},"reference":[{"issue":"1","key":"2026093009082771600_cit1","doi-asserted-by":"publisher","first-page":"8","DOI":"10.1038\/s41467-021-27909-x","article-title":"On the importance of\nthe electric double layer structure in aqueous electrocatalysis","volume":"13","author":"Shin","year":"2022","journal-title":"Nat. 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