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Realizing such molecular\u2010level differentiation requires stringent control over mean pore size, pore uniformity, and the nature of the surface charge of the membrane. However, this remains a bottleneck in conventional thin\u2010film composite membranes due to their structural limitations, as a outcome of the interfacial polymerization at a single liquid\u2010liquid interface. Here, a surfactant\u2010mediated multi\u2010stage interfacial polymerization forming a tri\u2010layer polyamide nanofilm with structural heterogeneity along its thickness in the form of a composite membrane is reported. This tri\u2010layer structure is formed as a mould of the liquid\u2010liquid interface defined by three distinct reaction zones with two sub\u2010interfaces. The multi\u2010stage interfacial polymerization enables precise control over the thickness, degree of crosslinking, and the mean pore size of the nanofilms. The resulting nanofilm composite membranes show high methanol permeance (8.3 Lm\n                    <jats:sup>\u22122<\/jats:sup>\n                    h\n                    <jats:sup>\u22121<\/jats:sup>\n                    bar\n                    <jats:sup>\u22121<\/jats:sup>\n                    ), efficient methanol\u2010rich mixed solvent separation, and precise molecular differentiation between two similar\u2010sized molecules (azobenzene and neutral red) with an extremely high selectivity of &gt;480. This selectivity surpasses that of state\u2010of\u2010the\u2010art organic\u2010solvent\u2010nanofiltration membranes (OSN). The combination of outstanding separation performance and scalable fabrication establishes a strategy for the rational design of application\u2010specific OSN membranes.\n                  <\/jats:p>","DOI":"10.1002\/adma.74320","type":"journal-article","created":{"date-parts":[[2026,7,29]],"date-time":"2026-07-29T08:12:48Z","timestamp":1785312768000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":0,"title":["Realizing Precise Molecular Differentiation in Heterogeneous Polyamide Nanofilms Formed via Multi\u2010Stage Interfacial Polymerization"],"prefix":"10.1002","volume":"38","author":[{"ORCID":"https:\/\/orcid.org\/0009-0004-1786-2974","authenticated-orcid":false,"given":"Manas Ranjan","family":"Puhan","sequence":"first","affiliation":[{"name":"Membrane Science and Separation Technology Division CSIR\u2010Central Salt and Marine Chemicals Research Institute G.B. 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