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Herein, a functional nanofilm was prepared via an interfacially confined condensation strategy, using tetraphenylaldehyde (TFPE) and acylhydrazide derivatives as the building blocks. Incorporating electron-withdrawing cyano moieties into the acylhydrazone backbone enables the simultaneous formation of both dynamic C\u2550N bonds and conjugated C\u2550C bonds within a single conjugated framework. The designed asymmetric building block, a 1,4-phenylene linker bearing an acylhydrazide and a cyanomethyl group at the para positions, effectively modulates \u03c0-electron delocalization and creates cyano-enriched N2H4-reactive sites in the conjugated donor\u2013acceptor (D-A) system, thereby promoting intramolecular charge transfer (ICT) and producing a large Stokes shift. These structural features also significantly influence the fluorescence turn-off sensing of the obtained nanofilms for gaseous N2H4. Performance screening identifies the heterostructural TFPE-CN nanofilm as the optimal candidate, featuring a free-standing, defect-free morphology, a favorable photoluminescence quantum yield of 30.8%, and exceptional stability. Integrated into a home-built portable sensing platform, the TFPE-CN nanofilm enables real-time, in situ detection of N2H4 vapor, delivering ultrahigh sensitivity (detection limit \u2248 130 ppt), rapid response (&amp;lt;11 s), excellent selectivity, and robust stability. This work offers an asymmetric molecular engineering strategy for fabricating interfacial nanofilms and lays a foundation for developing high-performance and portable sensing platforms for N2H4 vapor.<\/jats:p>","DOI":"10.1021\/acs.analchem.6c03767","type":"journal-article","created":{"date-parts":[[2026,9,1]],"date-time":"2026-09-01T16:04:50Z","timestamp":1788278690000},"page":"26001-26011","source":"Crossref","is-referenced-by-count":0,"title":["Heterostructural\nCyano-Functionalized Nanofilm Sensors\nvia Interfacially Confined Dynamic Condensation toward High-Performance\nHydrazine Vapor Detection"],"prefix":"10.1021","volume":"98","author":[{"given":"Jianyu","family":"Tuo","sequence":"first","affiliation":[{"name":"Shaanxi Normal University , , ,","place":["Xi\u2019an, P. R. China, 710119"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Yong","family":"Chen","sequence":"additional","affiliation":[{"name":"Shaanxi Normal University , , ,","place":["Xi\u2019an, P. R. China, 710119"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-8284-6496","authenticated-orcid":true,"given":"Kaixiang","family":"Cui","sequence":"additional","affiliation":[{"name":"Shaanxi Normal University , , ,","place":["Xi\u2019an, P. R. China, 710119"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Ruijuan","family":"Wen","sequence":"additional","affiliation":[{"name":"Shaanxi Normal University , , ,","place":["Xi\u2019an, P. R. China, 710119"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-9600-1045","authenticated-orcid":true,"given":"Taihong","family":"Liu","sequence":"additional","affiliation":[{"name":"Shaanxi Normal University , , ,","place":["Xi\u2019an, P. R. 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