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Adsorption of CTAB on Hydrophilic Silica Studied by Linear and Nonlinear Optical Spectroscopy

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Department of Chemistry, Durham University, South Road, Durham, DH1 3LE, United Kingdom
[email protected]
†Dept. of Chemistry, Surface Chemistry, Royal Institute of Technology, Drottning Kristinas Väg 51, SE-100 44 Stockholm, Sweden and YKI, Institute for Surface Chemistry, Stockholm, Sweden.
Cite this: J. Am. Chem. Soc. 2008, 130, 51, 17434–17445
Publication Date (Web):November 20, 2008
https://doi.org/10.1021/ja805169z
Copyright © 2008 American Chemical Society
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    Abstract

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    Vibrational sum-frequency spectroscopy (SFS) and total internal reflection Raman scattering (TIR Raman) have been used to study the adsorption of hexadecyltrimethylammonium bromide (CTAB) to hydrophilic silica. These two complementary techniques permit the determination of the adsorbed amount with a sensitivity of ∼1% of the maximum surface coverage, changes in the average tilt of the adsorbed molecules, the presence of asymmetric aggregates in the adsorbed film, and the structure and orientation of the water molecules in the interfacial region. The TIR Raman spectra show a monotonic increase with CTAB concentration with no measurable changes in the relative intensities of the different polarization combinations probed, implying that no significant changes occur in the conformational order of the hydrocarbon chain. In the sum-frequency (SF) spectra, no detectable peaks from the surfactant headgroup and hydrophobic chain were observed at any surface coverage. Major changes are observed in the water bands of the SF spectra, as the originally negatively charged silica surface becomes positively charged with an increase in the adsorbed amount, inducing a change in the polar orientation of the water molecules near the surface. The detection limits for hydrocarbons chains in the SF spectra were estimated by comparison with the SF spectrum of a disordered octadecyltrichlorosilane monolayer. The simulations demonstrate that the asymmetry in the adsorbed CTAB layer at any concentration is less than 5% of a monolayer. The results obtained pose severe constraints on the possible structural models, in particular at concentrations below the critical micellar concentration where information is scarce. The formation of hemimicelles, monolayers and other asymmetric aggregates is ruled out, with centrosymmetric aggregates forming from early on in the adsorption process.

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    2-D Correlation analysis of trimethyl ammonium vibrational modes in Raman spectra; fitting parameters for SF spectra; selected sum-frequency spectra collected under the PPP and SPS polarization; enlarged SSP spectra. This material is available free of charge via the Internet at http://pubs.acs.org.

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