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This study shows that films based on the non\u2010fullerene acceptor Y6 can be precisely structured via assembly at the air\u2010water interface. Theoretical cross\u2010sectional areas, Langmuir isotherms, and Brewster angle microscopy reveal that Y6, despite its complex structure, is sufficiently amphiphilic to form well\u2010defined 2D\u00a0layers. Mechanical annealing through repeated compression\u2010expansion cycles systematically improves structural uniformity, as evidenced by narrower in situ detected fluorescence spectra, while simultaneously shifting the maximum of the compressional modulus toward denser packing. Compared to spin\u2010cast films, Langmuir\u2013Schaefer (LS) layers exhibit a significantly reduced Stokes shift, suggesting less reorganization after photoexcitation and thus a higher supramolecular order. Organic thin\u2010film transistors (OTFTs) fabricated using the LS technique achieve mobilities comparable to those of spin\u2010cast films, despite being substantially thinner (\u2264\u00a03\u00a0nm, determined by atomic force microscopy), thus requiring considerably less material. Notably, Y6\u2010LS OTFTs outperform previously reported polymer\u2010based LS\u2010OTFTs by one order of magnitude in charge carrier mobility. This work highlights the potential of interfacial assembly for thin film fabrication and underscores the advantages of mechanical annealing and in situ spectroscopy to enhance the performance of organic optoelectronic devices.<\/jats:p>","DOI":"10.1002\/adma.202509825","type":"journal-article","created":{"date-parts":[[2025,11,10]],"date-time":"2025-11-10T09:48:13Z","timestamp":1762768093000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":2,"title":["Quasi\u20102D Morphologies of a Non\u2010Fullerene Acceptor Y6 by Interfacial Assembly via Langmuir\u2013Schaefer Technique"],"prefix":"10.1002","volume":"38","author":[{"ORCID":"https:\/\/orcid.org\/0009-0002-4930-6935","authenticated-orcid":false,"given":"Yisak Tsegazab","family":"Gerase","sequence":"first","affiliation":[{"name":"Institute of Physical Chemistry Friedrich Schiller University Jena  Helmholtzweg 4 07743 Jena Germany"},{"name":"Leibniz Institute of Photonic Technology (IPHT)  Albert\u2010Einstein\u2010Str. 9 07745 Jena Germany"}],"role":[{"role":"author","vocabulary":"crossref"}]},{"given":"Anna","family":"Elmanova","sequence":"additional","affiliation":[{"name":"Institute of Physical Chemistry Friedrich Schiller University Jena  Helmholtzweg 4 07743 Jena Germany"},{"name":"Leibniz Institute of Photonic Technology (IPHT)  Albert\u2010Einstein\u2010Str. 9 07745 Jena Germany"},{"name":"Sciclus GmbH &amp; Co. 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