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Nanoporous membranes prepared by supramolecular assembly of block copolymers have attracted increasing attention for their well-defined nanostructure, adjustable pore size, and large-scale manufacturing. In this context, the development of nanoporous membranes with tailored surface chemistry and specific functionalities presents significant opportunities and is critical for their practical applications. Herein, we demonstrate an efficient supramolecular approach for fabricating arginine-functionalized multifunctional nanoporous membranes by assembling the conventional polystyrene-block-poly(4-vinylpyridine) (PS-b-P4VP) with the designed arginine-based amphiphile containing three terminal pyrrole moieties (Py 3 -Arg) that could be polymerized to form the stable membranes in organic solvents followed by the removal of PS-b-P4VP template. Because of the distinct chemical properties of arginine moieties decorated on the wall surface, the obtained nanoporous membranes exhibit multifunctionality and hold a broad scope of promising applications, including but not limited to pH-tunable gating, selective adsorption, and membrane catalytic capability.

Block copolymers (BCPs) have enduring appeal for its intriguing assembly behaviors. Nevertheless, the unsatisfactory mechanical properties of BCPs make it a problem to fabricate freestanding membranes and hindered practical applications. Herein, a freestanding membrane with tunable pore size is prepared simply by co‐assembly of BCPs and subnanometer nanowires (SNWs), combining the abundant function of BCPs and prominent mechanical properties of SNWs. Benefited from synergy of the components and the hierarchical structure, the tensile strength of composite membrane is promoted by two orders of magnitude compared to that of BCPs. With the columnar pores aligning vertically to surfaces and the pore size regulated by processing conditions, the membranes exhibit precise size‐selected effect in ultrafiltration of Au nanoparticles (Au NPs) and can distinct NPs with diameter difference as tiny as 5 nm, demonstrating the promising prospect in separation technology and even widespread fields.

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