Issue 8, 2005
From the journal:

Physical Chemistry Chemical Physics

In situNMR and XRD studies of the growth mechanism of SBA-1†

C. C. Egger,‡a   M. W. Anderson,*a   G. J. T. Tiddyb  and  J. L. Cascic  

* Corresponding authors

a Department of Chemistry, UMIST, Manchester, UK
E-mail: m.anderson@manchester.ac.uk
Fax: +44 161 200 4559
Tel: +44 161 200 4517

b Department of Chemical Engineering, UMIST, Manchester, UK

c Synetix, Johnson Matthey, Billingham, UK

Abstract

In situ 17O, 14N and 29Si nuclear magnetic resonance (NMR) coupled with in situ energy dispersive X-ray diffraction (EDXRD) have been used to investigate the growth of the siliceous mesoporous material, SBA-1, synthesised under acidic conditions from a micellar solution of the surfactant hexadecyltriethylammonium bromide (HTEAB) and tetraethylorthosilicate (TEOS). For the last decade, the mechanism of growth of such materials has been thought to be driven by electrostatic interactions described as a co-assembly process between the silica species (I+) and the micelles (S+X−). However, this postulated model referred to as the “charge density matching model” has never been fully supported by experimental data for the acidic syntheses. We have carried out a detailed in situ study which challenges the so-called S+X−I+ pathway and instead suggests that a salting-out effect coupled with a drastic change in the water activity are responsible for the composite I13 (SBA-1 space group Pm[3 with combining macron]n) mesophase precipitation. Substantial reorganisation of the precipitated phase then results in the final structure.

Graphical abstract: In situ NMR and XRD studies of the growth mechanism of SBA-1

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Article information

DOI
https://doi.org/10.1039/B419293C
Article type
Paper
Submitted
23 Dec 2004
Accepted
16 Feb 2005
First published
17 Mar 2005

Phys. Chem. Chem. Phys., 2005,7, 1845-1855

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In situ NMR and XRD studies of the growth mechanism of SBA-1

C. C. Egger, M. W. Anderson, G. J. T. Tiddy and J. L. Casci, Phys. Chem. Chem. Phys., 2005, 7, 1845 DOI: 10.1039/B419293C

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