Synthesis of mesostructured silica from monoalkyl-substituted double five-ring units

Atsushi Shimojima; Hideki Kuge; Kazuyuki Kuroda

doi:10.1007/s10971-010-2224-7

Synthesis of mesostructured silica from monoalkyl-substituted double five-ring units

Atsushi Shimojima^*, Hideki Kuge, Kazuyuki Kuroda

^*Corresponding author for this work

Research output: Contribution to journal › Article › peer-review

15 Citations (Scopus)

Abstract

A mesostructured silica-based material was synthesized by self-assembly of a novel amphiphilic molecule consisting of a well-defined siloxane head with a double five-ring (D5R) structure and a hydrophobic alkyl tail. A precursor functionalized with ethoxy groups, C₂₂H₄₅Si ₁₀O₁₅(OEt)₉ (1), was hydrolyzed under an acidic condition with the retention of the D5R units, leading to the formation of two-dimensional (2D) hexagonal phase by evaporation-induced self-assembly of amphiphilic hydrolyzed molecules. Solid-state ²⁹Si MAS NMR analysis of the resulting hybrid solid confirmed that the D5R units were cross-linked to form siloxane networks. Calcination of this hybrid solid gave mesoporous silica with high BET surface area (740 m² g^-1). These results expand the design possibility of silica-based materials at both molecular- and meso-scales, leading to the bottom up synthesis of hierarchically ordered materials.

Original language	English
Pages (from-to)	263-268
Number of pages	6
Journal	Journal of Sol-Gel Science and Technology
Volume	57
Issue number	3
DOIs	https://doi.org/10.1007/s10971-010-2224-7
Publication status	Published - 2011 Mar
Externally published	Yes

Keywords

Mesoporous silica
Organic-inorganic hybrid
Self-assembly
Siloxane cage

ASJC Scopus subject areas

Electronic, Optical and Magnetic Materials
Ceramics and Composites
Chemistry(all)
Biomaterials
Condensed Matter Physics
Materials Chemistry

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10.1007/s10971-010-2224-7

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title = "Synthesis of mesostructured silica from monoalkyl-substituted double five-ring units",

abstract = "A mesostructured silica-based material was synthesized by self-assembly of a novel amphiphilic molecule consisting of a well-defined siloxane head with a double five-ring (D5R) structure and a hydrophobic alkyl tail. A precursor functionalized with ethoxy groups, C22H45Si 10O15(OEt)9 (1), was hydrolyzed under an acidic condition with the retention of the D5R units, leading to the formation of two-dimensional (2D) hexagonal phase by evaporation-induced self-assembly of amphiphilic hydrolyzed molecules. Solid-state 29Si MAS NMR analysis of the resulting hybrid solid confirmed that the D5R units were cross-linked to form siloxane networks. Calcination of this hybrid solid gave mesoporous silica with high BET surface area (740 m2 g-1). These results expand the design possibility of silica-based materials at both molecular- and meso-scales, leading to the bottom up synthesis of hierarchically ordered materials.",

keywords = "Mesoporous silica, Organic-inorganic hybrid, Self-assembly, Siloxane cage",

author = "Atsushi Shimojima and Hideki Kuge and Kazuyuki Kuroda",

note = "Funding Information: Acknowledgments The authors are grateful to Prof. D. Mochizuki (Tokyo Institute of Technology), Dr. Y. Hagiwara, and Mr. R. Goto (Waseda University) for experimental help. This work was supported in part by the Elements Science and Technology Project of the Ministry of Education, Culture, Sports, Science and Technology (MEXT) of Japan, and a Waseda University Grant for Special Research Projects (No. 2009B-172). This work was performed under the Global COE program {\textquoteleft}{\textquoteleft}Practical Chemical Wisdom{\textquoteright}{\textquoteright}. The A3 Foresight Program {\textquoteleft}{\textquoteleft}Synthesis and Structural Resolution of Novel Mesoporous Materials{\textquoteright}{\textquoteright} supported by the Japan Society for the Promotion of Science (JSPS) is greatly appreciated.",

year = "2011",

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doi = "10.1007/s10971-010-2224-7",

language = "English",

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journal = "Journal of Sol-Gel Science and Technology",

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AU - Shimojima, Atsushi

AU - Kuge, Hideki

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N1 - Funding Information: Acknowledgments The authors are grateful to Prof. D. Mochizuki (Tokyo Institute of Technology), Dr. Y. Hagiwara, and Mr. R. Goto (Waseda University) for experimental help. This work was supported in part by the Elements Science and Technology Project of the Ministry of Education, Culture, Sports, Science and Technology (MEXT) of Japan, and a Waseda University Grant for Special Research Projects (No. 2009B-172). This work was performed under the Global COE program ‘‘Practical Chemical Wisdom’’. The A3 Foresight Program ‘‘Synthesis and Structural Resolution of Novel Mesoporous Materials’’ supported by the Japan Society for the Promotion of Science (JSPS) is greatly appreciated.

PY - 2011/3

Y1 - 2011/3

N2 - A mesostructured silica-based material was synthesized by self-assembly of a novel amphiphilic molecule consisting of a well-defined siloxane head with a double five-ring (D5R) structure and a hydrophobic alkyl tail. A precursor functionalized with ethoxy groups, C22H45Si 10O15(OEt)9 (1), was hydrolyzed under an acidic condition with the retention of the D5R units, leading to the formation of two-dimensional (2D) hexagonal phase by evaporation-induced self-assembly of amphiphilic hydrolyzed molecules. Solid-state 29Si MAS NMR analysis of the resulting hybrid solid confirmed that the D5R units were cross-linked to form siloxane networks. Calcination of this hybrid solid gave mesoporous silica with high BET surface area (740 m2 g-1). These results expand the design possibility of silica-based materials at both molecular- and meso-scales, leading to the bottom up synthesis of hierarchically ordered materials.

AB - A mesostructured silica-based material was synthesized by self-assembly of a novel amphiphilic molecule consisting of a well-defined siloxane head with a double five-ring (D5R) structure and a hydrophobic alkyl tail. A precursor functionalized with ethoxy groups, C22H45Si 10O15(OEt)9 (1), was hydrolyzed under an acidic condition with the retention of the D5R units, leading to the formation of two-dimensional (2D) hexagonal phase by evaporation-induced self-assembly of amphiphilic hydrolyzed molecules. Solid-state 29Si MAS NMR analysis of the resulting hybrid solid confirmed that the D5R units were cross-linked to form siloxane networks. Calcination of this hybrid solid gave mesoporous silica with high BET surface area (740 m2 g-1). These results expand the design possibility of silica-based materials at both molecular- and meso-scales, leading to the bottom up synthesis of hierarchically ordered materials.

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Synthesis of mesostructured silica from monoalkyl-substituted double five-ring units

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