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Monitoring Silane Sol-Gel Kinetics with In-Situ Optical Turbidity Scanning and Dynamic Light Scattering

Department of Biological Engineering, Utah State University, Logan, UT 84322-4105, USA
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Author to whom correspondence should be addressed.
Molecules 2019, 24(16), 2931; https://doi.org/10.3390/molecules24162931
Received: 13 June 2019 / Revised: 29 July 2019 / Accepted: 2 August 2019 / Published: 13 August 2019
(This article belongs to the Special Issue Sol-Gel Chemistry. From Molecule to Functional Materials)
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Abstract

Organosilanes (e.g., R’-SiOR3) provide hydrophobic functionality in thin-film coatings, porous gels, and particles. Compared with tetraalkoxysilanes (SiOR4), organosilanes exhibit distinct reaction kinetics and assembly mechanisms arising from steric and electronic properties of the R’ group on the silicon atom. Here, the hydrolysis and condensation pathways of n-propyltrimethoxy silane (nPM) and a tri-fluorinated analog of nPM, 3,3,3-trifluoropropyl trimethoxy silane (3F), were investigated under aqueous conditions at pH 1.7, 2.0, 3.0, and 4.0. Prior to hydrolysis, 3F and nPM are insoluble in water and form a lens at the bottom (3F) or top (nPM) of the solutions. This phase separation was employed to follow reaction kinetics using a Turbiscan instrument to monitor hydrolysis through solubilization of the neat silane lens while simultaneously tracking condensation-induced turbidity throughout the bulk solution. Dynamic light scattering confirmed the silane condensation and particle aggregation processes reported by the turbidity scanning. Employing macroscopic phase separation of the starting reactants from the solvent further allows for control over the reaction kinetics, as the interfacial area can be readily controlled by reaction vessel geometry, namely by controlling the surface area to volume. In-situ turbidity scanning and dynamic light scattering revealed distinct reaction kinetics for nPM and 3F, attributable to the electron withdrawing and donating nature of the fluoro- and organo-side chains of 3F and nPM, respectively. View Full-Text
Keywords: organosilane; fluorosilane; ORMOSIL; hydrophobic nanoparticle; aqueous sol-gel synthesis; Turbiscan organosilane; fluorosilane; ORMOSIL; hydrophobic nanoparticle; aqueous sol-gel synthesis; Turbiscan
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Giasuddin, A.B.M.; Britt, D.W. Monitoring Silane Sol-Gel Kinetics with In-Situ Optical Turbidity Scanning and Dynamic Light Scattering. Molecules 2019, 24, 2931.

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