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Deposition of Dense Siloxane Monolayers from Water and Trimethoxyorganosilane Vapor

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Randall D. Lowe†, Matthew A. Pellow‡, T. Daniel P. Stack‡, and Christopher E. D. Chidsey*‡

^†Department of Chemical Engineering and ^‡Department of Chemistry, Stanford University, Stanford, California 94305, United States

Langmuir, 2011, 27 (16), pp 9928–9935

DOI: 10.1021/la201333y

Publication Date (Web): July 1, 2011

E-mail: chidsey@stanford.edu.

Section:

Surface Chemistry and Colloids

Abstract

A convenient, laboratory-scale method for the vapor deposition of dense siloxane monolayers onto oxide substrates was demonstrated. This method was studied and optimized at 110 °C under reduced pressure with the vapor of tetradecyltris(deuteromethoxy)silane, (CD₃O)₃Si(CH₂)₁₃CH₃, and water from the dehydration of MgSO₄·7H₂O. Ellipsometric thicknesses, water contact angles, Fourier transform infrared (FTIR) spectroscopy, and electrochemical capacitance measurements were used to probe monolayer densification. The CD₃ stretching mode in the FTIR spectrum was monitored as a function of the deposition time and amounts of silane and water reactants. This method probed the unhydrolyzed methoxy groups on adsorbed silanes. Excess silane and water were necessary to achieve dense, completely hydrolyzed monolayers. In the presence of sufficient silane, an excess of water above the calculated stoichiometric amount was necessary to hydrolyze all methoxy groups and achieve dense monolayers. The excess water was partially attributed to the reversibility of the hydrolysis of the methoxy groups.

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History

Published In Issue August 16, 2011
Article ASAPJuly 22, 2011
Just Accepted ManuscriptJuly 01, 2011
Received: April 12, 2011
Revised: June 29, 2011

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Article

Deposition of Dense Siloxane Monolayers from Water and Trimethoxyorganosilane Vapor

Abstract