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We systematically examined swelling and delamination behaviors of platelet single crystals of protonated layered metal oxides with a series of tetraalkylammonium (TAA) hydroxide solutions. Upon contact with the solutions, the crystals immediately underwent massive expansion by several tens to hundreds of times. The swollen crystals could be delaminated into elementary layers by the application of external shear force. The exfoliation behavior was dependent on TAA ions, especially in terms of yield and lateral size/shape of the delaminated nanosheets. The swollen crystals with TAA ions with longer alkyl chains were delaminated almost completely, but irregular and fractured small sheets were yielded. Such long alkyl chains become entangled on the oxide layer and resulting hydrophobic interactions may be responsible for the lateral fragmentation. We found that replacement of aqueous solutions with organic solvents to suppress the hydrophobic interactions is effective to produce the oversized nanosheets in rectangular shape with sharp edges.

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  This is the peer reviewed version of the following article: Y. Song, N. Sakai, Y. Ebina, N. Iyi, T. Kikuchi, R. Ma, Y. Ishida, T. Sasaki, Systematic Study on Swelling/Delamination of Layered Metal Oxides with Quaternary Ammonium Ions: Production of Well-Shaped/Oversized Unilamellar Nanosheets. Small Methods 2025, 9, 2401055, which has been published in final form at https://doi.org/10.1002/smtd.202401055. This article may be used for non-commercial purposes in accordance with Wiley Terms and Conditions for Use of Self-Archived Versions. This article may not be enhanced, enriched or otherwise transformed into a derivative work, without express permission from Wiley or by statutory rights under applicable legislation. Copyright notices must not be removed, obscured or modified. The article must be linked to Wiley’s version of record on Wiley Online Library and any embedding, framing or otherwise making available the article or pages thereof by third parties from platforms, services and websites other than Wiley Online Library must be prohibited.

Keyword: delamination, hydrophobic effect, intercalation, layered compounds, oversized high-quality nanosheets

Date published: 2024-09-16

Publisher: Wiley

Journal:

• Small Methods (ISSN: 23669608) vol. 9 issue. 3

Funding:

• Japan Science and Technology Agency JPMJCR22B1
• Japan Science and Technology Agency JPMJCR17N1

Manuscript type: Author's version (Accepted manuscript)

MDR DOI: https://doi.org/10.48505/nims.5380

First published URL: https://doi.org/10.1002/smtd.202401055

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Updated at: 2025-09-16 08:30:17 +0900

Published on MDR: 2025-09-16 08:19:10 +0900