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However, the thickness control of free-standing nanosheets composed of nonlayered compounds remains a fundamental challenge. Here, we report a solid-state surfactant templating strategy for synthesizing free-standing amorphous siloxane nanosheets with subnanometer thickness precision. By tailoring the length of ethylene oxide chains of the surfactant, we reproducibly obtained nanosheets with precisely defined thicknesses of 0.9, 1.5, 2.0, and 2.5 nm, while also enabling the incorporation of organofunctional groups into their frameworks. The resulting nanosheets exhibit thickness uniformity and high colloidal stability, enabling the formation of densely packed large-area films suitable for the systematic investigation of the properties, such as band gaps and breakdown strengths. We found that amorphous silica nanosheets showed exceptionally low overpotentials for the water dissociation reaction with a clear thickness dependence despite amorphous silica being widely regarded as a poor catalyst.<\/jats:p>","DOI":"10.1021\/acsnano.5c13829","type":"journal-article","created":{"date-parts":[[2025,11,4]],"date-time":"2025-11-04T15:40:01Z","timestamp":1762270801000},"page":"39936-39945","source":"Crossref","is-referenced-by-count":4,"title":["Surfactant\nTemplating for the Subnanometer Thickness\nEngineering of Free-Standing Nonlayered Nanosheets"],"prefix":"10.1021","volume":"19","author":[{"ORCID":"https:\/\/orcid.org\/0000-0001-5470-3826","authenticated-orcid":true,"given":"Eisuke","family":"Yamamoto","sequence":"first","affiliation":[{"name":"Nagoya University , , ,","place":["Nagoya, Japan, 464-8601"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Yuma","family":"Takezaki","sequence":"additional","affiliation":[{"name":"Nagoya University , , ,","place":["Nagoya, Japan, 464-8601"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Renjiro","family":"Hara","sequence":"additional","affiliation":[{"name":"Nagoya University , , ,","place":["Nagoya, Japan, 464-8601"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-6554-8400","authenticated-orcid":true,"given":"Makoto","family":"Kobayashi","sequence":"additional","affiliation":[{"name":"Nagoya University , , ,","place":["Nagoya, Japan, 464-8601"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-0595-0323","authenticated-orcid":true,"given":"Ruben","family":"Canton Vitoria","sequence":"additional","affiliation":[{"name":"Nagoya University , , ,","place":["Nagoya, Japan, 464-8601"]},{"name":"Osaka University , , ,","place":["Osaka, Japan, 567-0047"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-4414-655X","authenticated-orcid":true,"given":"Zixiao","family":"Shi","sequence":"additional","affiliation":[{"name":"Cornell University , , , ,","place":["Ithaca, New York, United States, 14853-2602"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"David A.","family":"Muller","sequence":"additional","affiliation":[{"name":"Cornell University , , , ,","place":["Ithaca, New York, United States, 14853-3501"]},{"name":"Kavli Institute at Cornell for Nanoscale Science , , ,","place":["Ithaca, New York, United States, 14853-2501"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-4599-4208","authenticated-orcid":true,"given":"Thomas E.","family":"Mallouk","sequence":"additional","affiliation":[{"name":"University of Pennsylvania , , , ,","place":["Philadelphia, Pennsylvania, United States, 19104-6323"]},{"name":"National Institute for Materials Science (NIMS) , , , ,","place":["Tsukuba, Ibaraki, Japan, 305-0044"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-6439-8068","authenticated-orcid":true,"given":"Minoru","family":"Osada","sequence":"additional","affiliation":[{"name":"Nagoya University , , ,","place":["Nagoya, Japan, 464-8601"]},{"name":"Nagoya University , , ,","place":["Nagoya, Japan, 464-8601"]}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"316","published-online":{"date-parts":[[2025,11,4]]},"reference":[{"key":"2026110402065895500_cit1","doi-asserted-by":"publisher","first-page":"1226419","DOI":"10.1126\/science.1226419","article-title":"Liquid\nExfoliation of Layered Materials","volume":"340","author":"Nicolosi","year":"2013","journal-title":"Science"},{"key":"2026110402065895500_cit2","doi-asserted-by":"publisher","first-page":"6225","DOI":"10.1021\/acs.chemrev.6b00558","article-title":"Recent Advances in Ultrathin Two-Dimensional\nNanomaterials","volume":"117","author":"Tan","year":"2017","journal-title":"Chem. 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Soc."},{"key":"2026110402065895500_cit43","doi-asserted-by":"publisher","first-page":"39","DOI":"10.3139\/113.110006","article-title":"Krafft Points\nand Cloud Points of Polyoxyethylated Nonionic Surfactants: Part 3\nThe Effect of Hydrotropes and other Organic Electrolytes","volume":"46","author":"Schott","year":"2009","journal-title":"Tenside, Surfactants, Deterg."},{"key":"2026110402065895500_cit44","doi-asserted-by":"publisher","first-page":"304","DOI":"10.1038\/416304a","article-title":"An Ordered Mesoporous\nOrganosilica Hybrid Material with a Crystal-like Wall Structure","volume":"416","author":"Inagaki","year":"2002","journal-title":"Nature"},{"key":"2026110402065895500_cit45","doi-asserted-by":"publisher","first-page":"5258","DOI":"10.1021\/ja9935862","article-title":"Evaporation-Induced\nSelf-Assembly of Hybrid Bridged\nSilsesquioxane Film and Particulate Mesophases with Integral Organic\nFunctionality","volume":"122","author":"Lu","year":"2000","journal-title":"J. Am. Chem. 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