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However, conventional etching techniques often struggle with the reproducible modulation of tip morphology, particularly the cone angle. In this work, we report a concentration gradient\u2010controlled electrochemical etching (CG\u2010CEE) strategy that facilitates the deterministic fabrication of carbon fiber nanoelectrodes with tailored geometries. By leveraging spatial confinement within a micro\u2010capillary sleeve to restrict etchant diffusion, CG\u2010CEE establishes a stable axial concentration gradient, enabling spatially regulated etching kinetics. Modulating the sleeve diameter allows for the precise adjustment of the concentration profile, thereby enabling the controlled fabrication of tip angles ranging from 6\u00b0 to 40\u00b0. This robust and highly reproducible method not only provides specialized nanoelectrodes for real\u2010time intracellular sensing but also exhibits exceptional versatility, as demonstrated by the fabrication of high\u2010precision tungsten needles. The CG\u2010CEE approach offers a powerful platform for the customized preparation of various nanotip electrodes in bioanalytical chemistry and micro\u2010fabrication.<\/jats:p>","DOI":"10.1002\/smtd.70723","type":"journal-article","created":{"date-parts":[[2026,5,22]],"date-time":"2026-05-22T04:52:12Z","timestamp":1779425532000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":1,"title":["Concentration Gradient\u2010Controlled Electrochemical Etching: A Universal Strategy for Nanoelectrodes with Tunable Geometries"],"prefix":"10.1002","volume":"10","author":[{"given":"Yaran","family":"Chang","sequence":"first","affiliation":[{"name":"State Key Laboratory of Materials Low\u2010Carbon Recycling Beijing Key Laboratory of Cardiopulmonary\u2010Cerebral Resuscitation Innovation and Translation Center of Excellence for Environmental Safety and Biological Effects Department of Chemistry College of Chemistry and Life Science Beijing 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