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Determination of structure-property relationships for 3-aminopropyltriethoxysilane films using x-ray reflectivity

Published online by Cambridge University Press:  03 April 2013

Sandip U. Argekar ,
Terence L. Kirley  and
Dale W. Schaefer
Sandip U. Argekar
Affiliation:
Chemical and Materials Engineering Programs, School of Energy, Environmental, Biological and Medical Engineering, University of Cincinnati, Cincinnati, Ohio 45221-0012
Terence L. Kirley
Affiliation:
Department of Pharmacology and Cell Biophysics, University of Cincinnati, Cincinnati, Ohio 45267-0575
Dale W. Schaefer*
Affiliation:
School of Energy, Environmental, Biological and Medical Engineering, University of Cincinnati, Cincinnati, Ohio 45221-0012
*
a)Address all correspondence to this author. e-mail: dale.schaefer@uc.edu
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Abstract

Films of 3-aminopropyltriethoxysilane films (APTES) deposited from nonpolar solvents show unusual hardness and tribological properties. The morphological origin of this behavior is determined using x-ray reflectivity. The deposited APTES films are smooth, evolving from a sparse structure when less than two-molecule-thick (<1 g/cm3) to a dense structure (1.26 g/cm3) when thicker. Previously reported improvements in wear resistance and hardness are due to the unusually dense nature of the APTES film. The density of multilayered APTES film has implications for its use as an interface-coupling agent because the film density limits the reactivity of embedded amine groups. A high-temperature cure (120 °C) does not affect film density but does significantly improve hydrolytic stability. Given their high density, predictable reactivity, stability and resistance to wear, multilayered APTES films are well suited for interfacial modification designed to improve mechanical properties, provided the films are properly cured.

Type
Articles
Information
Journal of Materials Research , Volume 28 , Issue 8 , 28 April 2013 , pp. 1118 - 1128
Copyright
Copyright © Materials Research Society 2013

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References

REFERENCES

Annaka, M., Yahiro, C., Nagase, K., Kikuchi, A., and Okano, T.: Real-time observation of coil-to-globule transition in thermosensitive poly(N-isopropylacrylamide) brushes by quartz crystal microbalance. Polymer 48(19), 5713 (2007).Google Scholar
Kim, J., Cho, J., Seidler, P.M., Kurland, N.E., and Yadavalli, V.K.: Investigations of chemical modifications of amino-terminated organic films on silicon substrates and controlled protein immobilization. Langmuir 26(4), 2599 (2010).Google Scholar
Zhang, Z.L., Crozatier, C., Le Berre, M., and Chen, Y.: In situ bio-functionalization and cell adhesion in microfluidic devices. Microelectron. Eng. 78–79, 556 (2005).Google Scholar
Ranieri, J.P., Bellamkonda, R., Jacob, J., Vargo, T.G., Gardella, J.A., and Aebischer, P.: Selective neuronal cell attachment to a covalently patterned monoamine on fluorinated ethylene propylene films. J. Biomed. Mater. Res. 27(7), 917 (1993).CrossRefGoogle ScholarPubMed
Bikiaris, D., Matzinos, P., Larena, A., Flaris, V., and Panayiotou, C.: Use of silane agents and poly(propylene-g-maleic anhydride) copolymer as adhesion promoters in glass fiber/polypropylene composites. J. Appl. Polym. Sci. 81(3), 701 (2001).Google Scholar
González-Benito, J.: The nature of the structural gradient in epoxy curing at a glass fiber/epoxy matrix interface using FTIR imaging. J. Colloid Interface Sci. 267(2), 326 (2003).Google Scholar
Kim, J.Y., Seidler, P., Wan, L.S., and Fill, C.: Formation, structure, and reactivity of amino-terminated organic films on silicon substrates. J. Colloid Interface Sci. 329(1), 114 (2009).Google Scholar
Vandenberg, E.T., Bertilsson, L., Liedberg, B., Uvdal, K., Erlandsson, R., Elwing, H., and Lundström, I.: Structure of 3-aminopropyl triethoxy silane on silicon oxide. J. Colloid Interface Sci. 147(1), 103 (1991).CrossRefGoogle Scholar
Wang, W. and Vaughn, M.W.: Morphology and amine accessibility of (3-aminopropyl) triethoxysilane films on glass surfaces. Scanning 30(2), 65 (2008).Google Scholar
Howarter, J.A. and Youngblood, J.P.: Optimization of silica silanization by 3-aminopropyltriethoxysilane. Langmuir 22(26), 11142 (2006).Google Scholar
Kim, J., Holinga, G.J., and Somorjai, G.A.: Curing induced structural reorganization and enhanced reactivity of amino-terminated organic thin films on solid substrates: Observations of two types of chemically and structurally unique amino groups on the surface. Langmuir 27(9), 5171 (2011).Google Scholar
Amemiya, Y., Hatakeyarna, A., and Shimamoto, N.: Aminosilane multilayer formed on a single-crystalline diamond surface with controlled nanoscopic hardness and bioactivity by a wet process. Langmuir 25(1), 203 (2009).Google Scholar
Gu, Q.L. and Cheng, X.H.: Tribological behaviors of self-assembled 3-aminopropyltriethoxysilane films on silicon. Curr. Appl. Phys. 8(5), 583 (2008).CrossRefGoogle Scholar
Dong, X., Wang, P., Argekar, S., and Schaefer, D.W.: Structure and composition of trivalent chromium process (TCP) films on Al alloy. Langmuir 26(13), 10833 (2010).Google Scholar
Heiney, P.A., Grüneberg, K., Fang, J., Dulcey, C., and Shashidhar, R.: Structure and growth of chromophore-functionalized (3-Aminopropyl)triethoxysilane self-assembled on silicon. Langmuir 16(6), 2651 (2000).Google Scholar
Simon, A., Cohen-Bouhacina, T., Porte, M.C., Aime, J.P., and Baquey, C.: Study of two grafting methods for obtaining a 3-aminopropyltriethoxysilane monolayer on silica surface. J. Colloid Interface Sci. 251(2), 278 (2002).CrossRefGoogle ScholarPubMed
Ilavsky, J. and Jemian, P.R.: Irena: Tool suite for modeling and analysis of small-angle scattering. J. Appl. Crystallogr. 42(2), 347 (2009).Google Scholar
Coussot, G., Perrin, C., Moreau, T., Dobrijevic, M., Le Postollec, A., and Vandenabeele-Trambouze, O.: A rapid and reversible colorimetric assay for the characterization of aminated solid surfaces. Anal. Bioanal. Chem. 399(3), 1061 (2011).Google Scholar
Kim, J., Seidler, P., Fill, C., and Wan, L.S.: Investigations of the effect of curing conditions on the structure and stability of amino-functionalized organic films on silicon substrates by fourier transform infrared spectroscopy, ellipsometry, and fluorescence microscopy. Surf. Sci. 602(21), 3323 (2008).CrossRefGoogle Scholar
Richter, A.G., Yu, C.J., Datta, A., Kmetko, J., and Dutta, P.: In situ and interrupted-growth studies of the self-assembly of octadecyltrichlorosilane monolayers. Phys. Rev. E: Stat. Nonlinear Soft Matter Phys. 61(1), 607 (2000).Google Scholar
Beari, F., Brand, M., Jenkner, P., Lehnert, R., Metternich, H.J., Monkiewicz, J., and Siesler, H.W.: Organofunctional alkoxysilanes in dilute aqueous solution: New accounts on the dynamic structural mutability. J. Organomet. Chem. 625(2), 208 (2001).Google Scholar
Wasserman, S.R., Whitesides, G.M., Tidswell, I.M., Ocko, B.M., Pershan, P.S., and Axe, J.D.: The structure of self-assembled monolayers of alkylsiloxanes on silicon: A comparison of results from ellipsometry and low-angle x-ray reflectivity. J. Am. Chem. Soc. 111(15), 5852 (1989).Google Scholar
Birkholz, M., Zaumseil, P., Kittler, M., Wallat, I., and Heyn, M.P.: Structure of biomembrane-on-silicon hybrids derived from x-ray reflectometry. Mater. Sci. Eng., B. 134(2–3), 125 (2006).Google Scholar
Vallée, C., Goullet, A., Granier, A., van der Lee, A., Durand, J., and Marlière, C.: Inorganic to organic crossover in thin films deposited from O2/TEOS plasmas. J. Non-Cryst. Solids 272(2–3), 163 (2000).Google Scholar
Bierbaum, K., Grunze, M., Baski, A.A., Chi, L.F., Schrepp, W., and Fuchs, H.: Growth of self-assembled n-alkyltrichlorosilane films on Si(100) investigated by atomic force microscopy. Langmuir 11(6), 2143 (1995).Google Scholar
Kellerman, B.K., Chason, E., Adams, D.P., Mayer, T.M., and White, J.M.: In-situ x-ray reflectivity investigation of growth and surface morphology evolution during Fe chemical vapor deposition on Si(001). Surf. Sci. 375(2–3), 331 (1997).Google Scholar
Wang, Y., Wang, P., Kohls, D., Hamilton, W.A., and Schaefer, D.W.: Water absorption and transport in bis-amino silane films, in Silanes and Other Coupling Agents, edited by Mittal, K.L. (VSP/Brill, Leiden, Netherlands, 2008), p. 95.Google Scholar
Jang, K. and Kim, H.: The gas barrier coating of 3-aminopropyltriethoxysilane on polypropylene film. J. Sol-Gel Sci. Technol. 41(1), 19 (2007).Google Scholar
Jang, L.S. and Liu, H.J.: Fabrication of protein chips based on 3-aminopropyltriethoxysilane as a monolayer. Biomed. Microdevices 11(2), 331 (2009).Google Scholar
Basarir, F. and Yoon, T.H.: Preparation of gamma-APS monolayer with complete coverage via contact printing. J. Colloid Interface Sci. 336(2), 393 (2009).Google Scholar
Metwalli, E., Haines, D., Becker, O., Conzone, S., and Pantano, C.G.: Surface characterizations of mono-, di-, and tri-aminosilane treated glass substrates. J. Colloid Interface Sci. 298(2), 825 (2006).Google Scholar