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There has been a spur on the precise fabrication of conventional planar SERS substrates with high performance and reproducibility. Common methods, such as ion beam and colloidal lithography, provide high\u2010quality substrates but are often limited by high costs, complex processes, and challenges associated with mass manufacturing. Triboelectrification\u2010driven self\u2010assembly of dry colloidal powder offers a promising dry approach to attain ordered monolayer colloidal particles in \u00a0s rapidly. Here, we use this approach to produce high\u2010performance SERS substrates with reproducible signals. By optimizing particle size and gold coating thickness, we found that self\u2010assembled 500 nm particles with a 50 and 65 nm Au layer achieved a maximum enhancement factor (EF) of 1 \u00d7 10, and limit of detection (LOD) of 33\u201336 nM, in our initial characterization study without coordinate translation. Compared with commercial substrates (Silmeco; Hamamatsu) under matched conditions, this corresponds to\u00a020\u201324 \u00d7 lower LOD (33\u201336 nM vs. 680\u2013800 nM) and\u00a010\u2013100 \u00d7 higher maximum EF. These results highlight triboelectrification's ability to efficiently and cost\u2010effectively produce homogeneous monolayers, offering a promising alternative to more complex or expensive methods and unlocking the opportunity for large\u2010scale SERS substrate production with biosensing, diagnostics, and chemical detection\u00a0applications.<\/jats:p>","DOI":"10.1002\/smtd.202501660","type":"journal-article","created":{"date-parts":[[2026,3,8]],"date-time":"2026-03-08T17:20:53Z","timestamp":1772990453000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":0,"title":["SERS Substrate Fabrication via Rapid Triboelectrification\u2010Driven Self\u2010Assembly of Close\u2010Packed Colloidal Monolayers"],"prefix":"10.1002","volume":"10","author":[{"ORCID":"https:\/\/orcid.org\/0000-0003-0543-6455","authenticated-orcid":false,"given":"Mehdi","family":"Feizpour","sequence":"first","affiliation":[{"name":"Department of Applied Physics and Photonics Vrije Universiteit Brussel Brussels Belgium"}],"role":[{"role":"author","vocabulary":"crossref"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-9653-1938","authenticated-orcid":false,"given":"Ignaas S. 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