Assessing extreme models of the Stober synthesis using transients under a range of initial composition

Kangtaek Lee; Jee Loon Look; Michael T. Harris; Alon V. McCormick

doi:10.1006/jcis.1997.5089

Assessing extreme models of the Stober synthesis using transients under a range of initial composition

Kangtaek Lee, Jee Loon Look, Michael T. Harris, Alon V. McCormick

Department of Chemical and Biomolecular Engineering

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

80 Citations (Scopus)

Abstract

²⁹Si-NMR, conductimetry, and photon correlation spectroscopy are used to monitor the temporal profile of intermediate concentrations in Stober synthesis (i.e., ammonia-catalyzed hydrolysis of tetraethoxysilane in a batch reactor). Extreme models of the process are assessed by examining the effect of initial composition on these transients (over a wider range of composition than attempted previously). The trends with initial composition suggest that the nucleation is rate-limited by the hydrolysis of the singly hydrolyzed monomer, the product of which probably phase separates. Moreover, the trends are consistent with the aggregation model discussed by G.H. Bogush and C.F. Zukoski (J. Colloid Interface Sci. 142, 1, 19 (1991) and by M.T. Harris (Ph.D. dissertation, Univ. of Tennessee, 1992). The trends are not consistent with a growth model without aggregation.

Original language	English
Pages (from-to)	78-88
Number of pages	11
Journal	Journal of Colloid and Interface Science
Volume	194
Issue number	1
DOIs	https://doi.org/10.1006/jcis.1997.5089
Publication status	Published - 1997 Oct 1

Bibliographical note

Funding Information:
We acknowledge the use of characterization facility of the Center for Interfacial Engineering at the University of Minnesota and support from the Office of Naval Research and the Office of Basic Energy Sciences, Material Sciences Division, U.S. Department of Energy. We also thank Dr. Arun N. Sathyagal for clarification of the figures.

All Science Journal Classification (ASJC) codes

Electronic, Optical and Magnetic Materials
Biomaterials
Surfaces, Coatings and Films
Colloid and Surface Chemistry

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abstract = "29Si-NMR, conductimetry, and photon correlation spectroscopy are used to monitor the temporal profile of intermediate concentrations in Stober synthesis (i.e., ammonia-catalyzed hydrolysis of tetraethoxysilane in a batch reactor). Extreme models of the process are assessed by examining the effect of initial composition on these transients (over a wider range of composition than attempted previously). The trends with initial composition suggest that the nucleation is rate-limited by the hydrolysis of the singly hydrolyzed monomer, the product of which probably phase separates. Moreover, the trends are consistent with the aggregation model discussed by G.H. Bogush and C.F. Zukoski (J. Colloid Interface Sci. 142, 1, 19 (1991) and by M.T. Harris (Ph.D. dissertation, Univ. of Tennessee, 1992). The trends are not consistent with a growth model without aggregation.",

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note = "Funding Information: We acknowledge the use of characterization facility of the Center for Interfacial Engineering at the University of Minnesota and support from the Office of Naval Research and the Office of Basic Energy Sciences, Material Sciences Division, U.S. Department of Energy. We also thank Dr. Arun N. Sathyagal for clarification of the figures.",

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N1 - Funding Information: We acknowledge the use of characterization facility of the Center for Interfacial Engineering at the University of Minnesota and support from the Office of Naval Research and the Office of Basic Energy Sciences, Material Sciences Division, U.S. Department of Energy. We also thank Dr. Arun N. Sathyagal for clarification of the figures.

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N2 - 29Si-NMR, conductimetry, and photon correlation spectroscopy are used to monitor the temporal profile of intermediate concentrations in Stober synthesis (i.e., ammonia-catalyzed hydrolysis of tetraethoxysilane in a batch reactor). Extreme models of the process are assessed by examining the effect of initial composition on these transients (over a wider range of composition than attempted previously). The trends with initial composition suggest that the nucleation is rate-limited by the hydrolysis of the singly hydrolyzed monomer, the product of which probably phase separates. Moreover, the trends are consistent with the aggregation model discussed by G.H. Bogush and C.F. Zukoski (J. Colloid Interface Sci. 142, 1, 19 (1991) and by M.T. Harris (Ph.D. dissertation, Univ. of Tennessee, 1992). The trends are not consistent with a growth model without aggregation.

AB - 29Si-NMR, conductimetry, and photon correlation spectroscopy are used to monitor the temporal profile of intermediate concentrations in Stober synthesis (i.e., ammonia-catalyzed hydrolysis of tetraethoxysilane in a batch reactor). Extreme models of the process are assessed by examining the effect of initial composition on these transients (over a wider range of composition than attempted previously). The trends with initial composition suggest that the nucleation is rate-limited by the hydrolysis of the singly hydrolyzed monomer, the product of which probably phase separates. Moreover, the trends are consistent with the aggregation model discussed by G.H. Bogush and C.F. Zukoski (J. Colloid Interface Sci. 142, 1, 19 (1991) and by M.T. Harris (Ph.D. dissertation, Univ. of Tennessee, 1992). The trends are not consistent with a growth model without aggregation.

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Assessing extreme models of the Stober synthesis using transients under a range of initial composition

Abstract

Bibliographical note

All Science Journal Classification (ASJC) codes

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