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Covalent organic frameworks (COFs) have shown advantages in efficient capturing and detecting of copper ions due to their large surface area, robust chemical stability, and high sensitivity, but most of them are hydrophobic, leading to the limitation in sensing copper ions in aqueous media. Herein, the design and synthesis of an sp<jats:sup>2<\/jats:sup>\u2010carbon conjugated COF (sp<jats:sup>2<\/jats:sup>\u2010TPE\u2010COF) are reported with surfactant\u2010assisted water dispersion for detecting traces of copper ions based on the photo\u2010induced electron transfer (PET) mechanism. Importantly, the olefin\u2010linked conjugated backbone of sp<jats:sup>2<\/jats:sup>\u2010TPE\u2010COF works as a signal amplified transducer for metal ion sensing. Notably, it is found that a surfactant\u2010assisted strategy can greatly enhance COF's dispersion in aqueous solution and finely modulate their sensitivity with a significantly improved <jats:italic>K<\/jats:italic><jats:sub>SV<\/jats:sub> to 15.15 \u00d7 10<jats:sup>4<\/jats:sup> <jats:sc>m<\/jats:sc><jats:sup>\u22121<\/jats:sup> in SDBS (sodium dodecyl benzene sulfonate) solution, the value of which is larger than that of a majority of COF\/MOF based sensors for copper ions. This research demonstrates the promise of surfactant modulated fully \u03c0\u2010conjugated COFs for sensing applications.<\/jats:p>","DOI":"10.1002\/smll.202200388","type":"journal-article","created":{"date-parts":[[2022,5,2]],"date-time":"2022-05-02T01:58:58Z","timestamp":1651456738000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":44,"title":["Surfactant\u2010Modulated a Highly Sensitive Fluorescent Probe of Fully Conjugated Covalent Organic Nanosheets for Detecting Copper Ions in Aqueous Solution"],"prefix":"10.1002","volume":"18","author":[{"given":"Zifeng","family":"Yan","sequence":"first","affiliation":[{"name":"Institute of Materials Research Shenzhen International Graduate School Tsinghua University  Shenzhen 518055 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Long","family":"Fang","sequence":"additional","affiliation":[{"name":"Key Laboratory for Polymeric Composite and Functional 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