A mechanistic study of the formation of mesoporous structures from in situ AC conductivity measurements

Alfonso E. Garcia-Bennett*, Ulrika Brohede, Robert P. Hodgkins, Niklas Hedin, Maria Strømme

*Corresponding author for this work

Research output: Contribution to journalArticle

12 Citations (Scopus)

Abstract

The purpose of this work is to study the kinetics of self-assembly in the formation mechanism of anionic templated mesoporous solids (AMS-n) during die first few seconds of the synthesis as well as to demonstrate the use of alternating ion current (AIC) conductivity measurements to follow the self-assembly in complex hybrid systems. The formation of different AMS-n caged-type mesostructures through the delayed addition of the silica source is demonstrated and explained in terms of the interaction between the co-structure-directing agent (CSDA) and the oppositely charged surfactant headgroup regions. Our findings, supported by transmission electron microscopy, 29Si magic angle spinning nuclear magnetic resonance (MAS NMR) spectroscopy, dynamic light scattering (DLS) measurements, and powder X-ray diffraction suggest that the interaction of the CSDA with the surfactant headgroup occurs within seconds after its addition to the synthesis gel leading to interaction between the polymerizing CSDAs and the oppositely charged micelle and to an increase in the micelle-CSDA aggregate size. Both DLS and AIC measurements agree that this process occurs within the first 1000 s after addition of the CSDA to the synthesis gel at room temperature. In addition to the mechanistic study it was found that the intermediate materials are comprised of a three-layer entity. Time-dependent 29Si MAS NMR studies reveal that an organo-silica layer forms around the micelles prior to a condensed outer inorganic shell of silica.

Original languageEnglish
Pages (from-to)9875-9881
Number of pages7
JournalLangmuir
Volume23
Issue number19
DOIs
Publication statusPublished - 11 Sep 2007
Externally publishedYes

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