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Morphology and Properties of Anti-Corrosion Organosilane Films

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Morphology and Properties of Anti-Corrosion Organosilane Films UNIVERSITY OF CINCINNATI Date:___________________ I, _________________________________________________________, hereby submit this work as part of the requirements for the degree of: in: It is entitled: This work and its defense approved by: Chair: _______________________________ _______________________________ _______________________________ _______________________________ _______________________________ Morphology and Properties of Anti-Corrosion Organosilane Films A dissertation submitted to the Division of Research and Advanced Studies of the University of Cincinnati in partial fulfillment of the requirements for the degree of DOCTOR OF PHILOSOPHY in the Department of Chemical and Materials Engineering of the College of Engineering 2006 by Guirong Pan B.S., Tongji University, P. R. China 1999 M.S. University of Cincinnati, Ohio, 2003 Committee Chair: Dr. Dale W. Schaefer Abstract Although it is known that certain organosilanes can dramatically improve the corrosion resistance when deposited on metals, the origin of this effect and its dependence on film characteristics are not fully understood. In this work, the morphology and structure of the silane films, as well as their response to water exposure, are studied mainly by neutron reflectivity. Hydrothermal conditioning and solvent swelling are used to challenge the films. The silanes studied include bis-[triethoxysilylpropyl]tetrasulfide (bis-sulfur) and bis- [trimethoxysilylpropyl]amine (bis-amino) as well as mixed silane films. Initial studies were done on films spin-coated on silicon wafer substrates from 1% solutions and cured at 80 °C. Here the focus is the effect of the bridging group on the morphology and water-barrier properties of the films. Subsequent work addresses the same systems deposited on aluminum substrates, films cured at 180 °C and films of larger thickness. The goal is to clarify the relationship between silane molecular structure, processing variables, morphology and water-barrier properties of films while developing a database for optimizing the performance in anti-corrosion applications. Bridging group is the key factor that controls the morphology and water-barrier properties of silane films. Bis-sulfur silane is not as condensed as bis-amino silane, but it swells less in water because of the hydrophobic nature of bridging group. By contrast, bis-amino film is more hydrophilic since the secondary amine group hydrogen bonds with water. The bulk mixed silane film swells with water to an extent that is slightly less than that of both components weighted by their volume fraction. But, based on the enhanced shrinkage that occurs upon water conditioning of the mixed film, condensation is accelerated in the mixed silane film. Bis-amino silane, may act as a catalyst in the hydrolysis of bis-sulfur silane leading to more ii silanols groups in the solution, which in turn will improve the wettability of the solution. This effect might explain the superior performance of the mixed film compared to pure bis-sulfur silane film. Processing variables also impact the water-barrier performance. For bis-sulfur silane films, both larger thickness and higher cure temperature are critical for effective water-barrier properties. iii iv Acknowledgements My deepest appreciation goes to my advisor, Dr. Dale W. Schaefer. I thank him for supervision, recommendations and suggestions during all these years involved in this challenging project. It is my great pleasure and honor to be Dr. Schaefer’s student. I extend my deep appreciation to Dr. Wim Van Ooij, for all his guidance and insights. I thank him for spending time serving as my committee. Sincere appreciation and gratitude are also to Dr. Greg Beaucage and Dr. Ray Y. Lin for their participation as my committee and their valuable insights and suggestions. Specially, I would like to thank Dr. Mike Kent at Sandia National Lab. Dr. Kent gave me enormous help with neutron reflectivity testing and data analysis. His guidance and advice is greatly appreciated. This project is funded by the Strategic Environmental Research and Development Program (www.serdp.org). This work benefited the use of Surface Profile Analysis Reflectometer (SPEAR) at Lujan Neutron Scattering Center at Los Alamos National Laboratory, NG7 reflectometer at National Institute of Standards and Technology (NIST) as well as POSYII at Argonne National lab. I thank Jaraslaw Majewski, Erik Watkins, Sushil Satija, v Young-Soo Seo, Rick Goyette and Jan Ilavsky for their effort in collecting the reflectivity data. I thank Professor James Boerio for use of the ellipsometer and AFM. I thank my lab mates (past and present: Kumar, Tingtai, Jian, Kim, Dazhi, Chetan, Kevin, Ryan, Yimin, Peng), members of SERDP group (Trilok, Chetan, Akshay) for their advice and help. I appreciate the support provided by the dedicated and enthusiastic staff members of Chemical and Materials Engineering Department and Chemistry Department. I would like to thank my dear friend Barbara M. Linder for providing her home for me to stay, and for her encouragement and support. To my friends Quanyan, Dan Wu, Li Guo, Bin Zheng, Feng Gao, Xuandong, Li Yuan, Shu Zheng who made my years at Cincinnati a pleasant experience. Special thanks to my husband Zhengsheng Li, for being there for me, for his encouragement, love and understanding throughout my studies. I am grateful to my family in China for their love, support and inspiration in all my endeavors. This work is dedicated to each and every of them. vi This dissertation is dedicated to My dear husband, parents and sister, for their love, caring, and support through the past years. vii Table of Contents ABSTRACT .................................................................................................................... II ACKNOWLEDGEMENTS...............................................................................................V TABLE OF CONTENTS.................................................................................................. 1 LIST OF FIGURES.......................................................................................................... 7 LIST OF TABLES ......................................................................................................... 15 LIST OF ABBREVIATIONS.......................................................................................... 16 CHAPTER 1. INTRODUCTION.................................................................................. 18 1.1 Research Significance and Objectives................................................................................. 18 1.2 Dissertation outline ............................................................................................................... 20 CHAPTER 2. LITERATURE REVIEW ....................................................................... 23 2.1. Corrosion Protection of Metals by Organosilane films.................................................... 23 2.1.1 Chemical structure of organosilanes..............................................................................................23 2.1.2. Silane solution chemistry: hydrolysis and condensation ..............................................................24 2.1.3 Processing Variables of Silanes in Solution ..................................................................................28 2.1.3.1 pH effect:................................................................................................................................28 2.1.3.2 Silane Concentration ..............................................................................................................29 1 2.1.3.3 Hydrolysis Time.....................................................................................................................30 2.1.3.4 The effect of metal substrate ..................................................................................................32 2.1.3.5 The Effect of Curing Step ......................................................................................................34 2.1.4 Structure Property Relationships in Corrosion-Inhibiting Films...................................................35 2.1.4.1 Interaction of silane with substrate.........................................................................................35 2.1.4.2 Interaction of water with silane..............................................................................................40 2.2. Neutron reflectivity.............................................................................................................. 41 2.2.1 History of Neutron (X-ray) reflectivity .........................................................................................41 2.2.2 Theory of Neutron (X-ray) reflectivity..........................................................................................43 2.2.2.1 Refractive Index .....................................................................................................................43 2.2.2.2 Snell’s law and Fresnel’s law.................................................................................................45 2.2.2.3 Reflectivity from a system with one interface........................................................................48 2.2.2.4 Reflectivity from a system with two parallel interfaces.........................................................50 2.2.2.5 Analysis of Reflectivity..........................................................................................................51 2.2.2.6
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