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Abstract The preparation of thin films of nanostructured functional materials is a critical step in a diverse array of applications ranging from photonics to separation science. New thin‐film fabrication methods are sought to harness the emerging potential of self‐assembled nanostructured materials as next‐generation membranes. Here, the authors show that nanometer‐scale control over the thickness of self‐assembled mesophases can be enacted by directional photopolymerization in the presence of highly photo‐attenuating molecular species. Metrology reveals average film growth rates below ten nanometers per second, indicating that high‐resolution fabrication is possible with this approach. The trends in experimental data are reproduced well in numerical simulations of mean‐field frontal photopolymerization modeled in a highly photo‐attenuating and photo‐bleaching medium. These simulation results connect the experimentally observed nanometer‐scale control of film growth to the strong photo‐attenuating nature of the mesophase, which originates from its high‐aromatic‐ring content. Water permeability measurements conducted on the fabricated thin films show the expected linear scaling of permeability with film thickness. Film permeabilities compare favorably with current state‐of‐the‐art nanofiltration and reverse osmosis membranes, suggesting that the current approach may be utilized to prepare new nanoporous membranes for such applications. 

Self-assembled membranes with uniform pore sizes tunable in 0.1-nm steps have been developed for organic solvent nanofiltration. 

Self-assembled materials are attractive for next-generation membranes. However, the need to align self-assembled nanostructures (e.g. cylinders, lamellae) and the narrow stability windows for ordered bicontinuous systems present serious challenges. We propose and demonstrate a novel approach that circumvents these challenges by exploiting size-selective transport in the water-continuous medium of a nanostructured polymer templated from a self-assembled lyotropic H 1 mesophase. Optimization of the mesophase composition enables high-fidelity retention of the H 1 structure on photoinduced cross-linking. The resulting material is a mechanically robust nanostructured polymer possessing internally and externally cross-linked nanofibrils surrounded by a continuous aqueous medium. Fabricated membranes show size selectivity at the 1- to 2-nm length scale and water permeabilities of ~10 liters m −2 hour −1 bar −1 μm. Moreover, the membranes display excellent antimicrobial properties due to the quaternary ammonium groups on the nanofibril surfaces. These results represent a breakthrough for the potential use of polymerized lyotropic mesophase membranes in practical water purification applications.