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Time-Resolved in Situ Small-Angle X-ray Scattering Study of Silica Particle Formation in Nonionic Water-in-Oil Microemulsions

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Department of Physical Chemistry and INSTM, Ca’ Foscari University of Venice, via Torino 155b, 30170 Venice, Italy, and Department of Chemistry and iNANO Interdisciplinary Nanoscience Center, University of Aarhus, Langelandsgade 140 DK-8000 Aarhus C, Denmark
* Corresponding author. E-mail: [email protected]. Fax: +39-0412346747.
†Ca’ Foscari University of Venice.
‡University of Aarhus.
Cite this: Langmuir 2008, 24, 10, 5225–5228
Publication Date (Web):April 23, 2008
Copyright © 2008 American Chemical Society

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    The formation of silica particles by the ammonia-catalyzed hydrolysis of tetraethyl orthosilicate (TEOS) in the polyoxyethylene (5) nonylphenyl ether (NP-5)/cyclohexane/water microemulsion system was investigated by time-resolved small-angle X-ray scattering (SAXS). The SAXS data could be modeled as a combination of two species where one describes the silica-particle containing microemulsion droplets and the other the reverse droplets. The analysis allowed the determination of the evolution of the system of particles of silica and reverse droplets. A model of nucleation and growth of the silica particles is confirmed and the volume fraction versus time data for the silica particles is in agreement with first order kinetics with respect to TEOS concentration. Moreover to describe the long time evolution of the system, a correlation among the silica particles has been taken into account by introducing a structure factor with a local silica volume fraction η = 0.1. This high local density is 2 orders of magnitude larger than the global silica fraction and can be explained in terms of depleting interaction.

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    Normalized distribution of the particle sizes for the sample after 78 h 45 min. TEM micrograph of silica particles after 10 h. Silica particle concentration versus time. Comparison between the SAXS measurement of two samples prepared in the absence of TEOS. The first sample contains the initial amount of cyclohexane, ammonia, and NP-5 with a water-to-surfactant ratio of R = 2.14 in the absence of ethanol. The second sample contains the same composition as the first with the addition of ethanol in a quantity that would correspond to that released upon the complete hydrolysis of TEOS. This material is available free of charge via the Internet at

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