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The clean energy future and lithium\u2010based energy storage systems heavily rely on highly efficient ionic separations. However, artificial recreation of such a sophisticated biostructure has been technically challenging. Here, a highly tunable design concept is introduced to fabricate monovalent ion\u2010selective membranes with asymmetric sub\u2010nanometer pores in which energy barriers are implanted. The energy barriers act against ionic movements, which hold the target ion while facilitating the transport of competing ions. The membrane consists of bilayer metal\u2010organic frameworks (MOF\u2010on\u2010MOF), possessing a 6 to 3.4\u2010angstrom passable cavity structure. The ionic current measurements exhibit an unprecedented ionic current rectification ratio of above 100 with exceptionally high selectivity ratios of 84 and 80 for K<jats:sup>+<\/jats:sup>\/Li<jats:sup>+<\/jats:sup> and Na<jats:sup>+<\/jats:sup>\/ Li<jats:sup>+<\/jats:sup>, respectively (1.14 Li<jats:sup>+<\/jats:sup> mol m<jats:sup>\u22122<\/jats:sup> h<jats:sup>\u22121<\/jats:sup>). Furthermore, using quantum mechanics\/molecular mechanics, it is shown that the combined effect of spatial hindrance and nucleophilic entrapment to induce energy surge baffles is responsible for the membrane's ultrahigh selectivity and ion rectification. This work demonstrates a striking advance in developing monovalent ion\u2010selective channels and has implications in sensing, energy storage, and separation technologies.<\/jats:p>","DOI":"10.1002\/adma.202107878","type":"journal-article","created":{"date-parts":[[2021,12,18]],"date-time":"2021-12-18T00:04:08Z","timestamp":1639785848000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":138,"title":["Designing Angstrom\u2010Scale Asymmetric MOF\u2010on\u2010MOF Cavities for High Monovalent Ion Selectivity"],"prefix":"10.1002","volume":"34","author":[{"given":"Mojtaba","family":"Abdollahzadeh","sequence":"first","affiliation":[{"name":"School of Engineering Macquarie University  Sydney NSW 2109 Australia"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Milton","family":"Chai","sequence":"additional","affiliation":[{"name":"School of Chemical Engineering University of Queensland  Brisbane QLD 4072 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