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Introduction to Surface-Initiated Atom Transfer Radical Polymerization and General Patterning Techniques

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Introduction to Surface-Initiated Atom Transfer Radical Polymerization and General Patterning Techniques Micro- and Nano-Structure of Polymers and Molecular Materials By Abdullah Mohammed M. Alswieleh DEPARTMENT OF CHEMISTRY UNIVERSITY OF SHEFFIELD A Thesis Submitted to the University of Sheffield for the Degree of Doctor of Philosophy July 2014 Declaration This thesis is submitted in fulfillment of the requirements of the degree of Doctor of Philosophy at the University of Sheffield. The work described in this thesis was undertaken between January 2011 and July 2014 under the supervision of Professor Graham Leggett and Professor Steven Armes. Unless otherwise stated, it is the work of the author and has not been submitted in whole or in part for any other degree at this or any other university or institution. July 2014 Signed: ……………………….. Abdullah Mohammed Alswieleh Department of Chemistry, Dainton Bulding, University of Sheffield, Brook Hill, Sheffield, UK. S3 7HF ii Acknowledgements For the duration of my PhD I have been fortunate enough to work with some truly talented, inspirational and friendly people. I would like to take this opportunity to say thank you to them: - I would like to thank Professor Graham Leggett and Professor Steven Armes, for giving me the unique opportunity of working in their research groups and for their advice and guidance throughout this project. - I would like to thank the University of Sheffield and everybody in chemistry department. I would like to thank GJL and SPA group members past and present, especially Alexander Johnson, Andrew Morse, Anna Tsargorodska, Ehtsham ul Haq, Irene Canton, Maria Cardellach, Mark Moxey, Mat Pringle, Nan Cheng, Omed Qadir, Osama El-Zubir, Paul Chapman, Peng Fan, Robert Ducker, Samson Patole, Sijing Xia, Vicki Cunningham, Vincent Ladmiral, Xuan Xue and Zhenyu Zhang. - I would like to thank all at the Kroto Research Institute, especially Claire Hurley. - I would like to thank King Saud University (KSU) in Riyadh for financial support for my PhD research. - Finally, I would like to thank all my family, my father, my mother and my brothers and sisters I couldn’t have done this without their support. Also, I do not forget my wife, I would not have been able to do this work without her. iii Publications 1- Alswieleh AM, Cheng N, Leggett GJ & Armes SP. Spatial control over crosslinking dictates the pH-responsive behavior of poly(2-(tert-butylamino)ethyl methacrylate) brushes. Langmuir, 2014, 30 (5), 1391–1400. 2- Alswieleh AM, Cheng N, Canton I, Ustbas B, Xue X, Ladmiral V, Xia S, Ducker RE, El Zubir O, Cartron ML, Hunter CN, Leggett GJ and Armes SP. Zwitterionic poly(amino acid methacrylate) brushes. J. Am. Chem. Soc, 2014, 136 (26), pp 9404–9413 3- Cunningham V, Alswieleh AM, Thompson K, Williams M, Leggett GJ, Armes SP, Musa O. Poly(glycerol monomethacrylate)-poly(benzyl methacrylate) diblock copolymer nanoparticles via RAFT emulsion polymerization: synthesis, characterization and interfacial activity. Macromolecules 2014, 47 (16), pp 5613–5623. 4- Blakeston AC, Alswieleh AM, Heath GR, Roth J, Bao P, Cheng N, Armes SP, Leggett GJ, Bushby RJ, Evans SD. A new poly(amino acid methacrylate) brush supports the formation of well-defined lipid membranes. In preparation. 5- ‘‘Spatial control over crosslinking affects the pH-responsive behavior of poly(2-(tert- butylamino)ethyl methacrylate) brushes’’ AM Alswieleh, SP Armes and GJ Leggett, Poster presentation at Soft Matter, Freiburg Institute of Advanced Studies, Germany, October 2013. 6- ‘‘Spatial control over crosslinking affects the pH-responsive behavior of poly(2-(tert- butylamino)ethyl methacrylate) brushes’’ AM Alswieleh, SP Armes and GJ Leggett, Poster presentation at 3rd Annual Postgraduate Symposium on Nanotechnology, the University of Birmingham, UK, December 2013. iv Contents Abbreviations....................................................................................................................xi List of Figures....................................................................................................................xiv List of Tables.....................................................................................................................xxv List of Schemes.................................................................................................................xxv Abstract ................................................................................................................................. - 1 - Chapter 1: Introduction ......................................................................................................... - 3 - 1.1 Self-Assembled Monolayers (SAMs) ......................................................................... - 3 - 1.1.1 SAMs of organosulfur derivatives ........................................................................ - 4 - 1.1.2 SAMs of organosilicon derivatives ...................................................................... - 6 - 1.2 Polymer brushes ........................................................................................................ - 10 - 1.2.1 Types of Polymer Brushes .................................................................................. - 11 - 1.2.1.1 Grafting To................................................................................................... - 11 - 1.2.1.2 Grafting From .............................................................................................. - 12 - 1.2.2 Atom transfer radical polymerization (ATRP) ................................................... - 14 - 1.2.3 Surface initiated atom transfer radical polymerization (SI-ATRP) .................... - 18 - 1.2.4 Stimulus-responsive polymer brushes ................................................................ - 22 - 1.2.4.1 Solvent-responsive polymer brushes ........................................................... - 23 - 1.2.4.2 pH- and ion-sensitive polymer brushes........................................................ - 24 - 1.3 Patterned SAMs and Polymer Brushes ..................................................................... - 26 - 1.3.1 Microcontact printing (µCP) .............................................................................. - 26 - 1.3.2 Photolithography ................................................................................................ - 28 - 1.3.2.1 Micro-scale UV lithography ........................................................................ - 29 - 1.3.2.2 Interferometric lithography .......................................................................... - 30 - 1.3.3 Electron beam lithography.................................................................................. - 33 - 1.3.4 Scanning probe lithography (SPL) ..................................................................... - 33 - 1.3.4.1 Scanning near-field optical microscopy (SNOM) ....................................... - 34 - v 1.3.4.2 Dip-pen lithography ..................................................................................... - 35 - 1.3.4.3 Local oxidation patterning ........................................................................... - 37 - 1.3.4.4 Mechanical surface patterning ..................................................................... - 37 - 1.4 Objectives and outline of the thesis........................................................................... - 38 - Chapter 2: Experimental ..................................................................................................... - 39 - 2.1 Materials .................................................................................................................... - 39 - 2.2 Cleaning glassware and substrates ............................................................................ - 40 - 2.3 Formation of self-assembled monolayers (SAMs).................................................... - 40 - 2.3.1 Silane initiator..................................................................................................... - 40 - 2.3.2 Thiol monolayers ............................................................................................... - 41 - 2.4 Sample handling ........................................................................................................ - 41 - 2.5 Surface characterizations........................................................................................... - 41 - 2.5.1 Contact angle measurements .............................................................................. - 41 - 2.5.1.1 Background .................................................................................................. - 41 - 2.5.1.2 Experimental procedure ............................................................................... - 42 - 2.5.2 Atomic Force Microscopy (AFM) ...................................................................... - 42 - 2.5.2.1 Introduction to AFM .................................................................................... - 42 - 2.5.2.2 Friction force microscopy (FFM) ................................................................ - 44 - 2.5.2.3 Experiment ................................................................................................... - 46 - 2.5.2.4 Image Acquisition ........................................................................................ - 46 - 2.5.3 Ellipsometry........................................................................................................ - 47 - 2.5.3.1 Background .................................................................................................
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