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The Pennsylvania State University the Graduate School College Of The Pennsylvania State University The Graduate School College of Engineering NOVEL TEMPLATE-LESS SYNTHESIS OF POLYCYANOACRYLATE NANOFIBERS A Thesis in Chemical Engineering by Pratik Mankidy 2007 Pratik Mankidy Submitted in Partial Fulfillment of the Requirements for the Degree of Doctor of Philosophy December 2007 The thesis of Pratik Mankidy was reviewed and approved* by the following: Henry C. Foley Professor of Chemical Engineering Thesis Advisor Chair of Committee Carlo G. Pantano Distinguished Professor of Materials Science and Engineering Janna K. Maranas Associate Professor of Chemical Engineering Andrew L. Zydney Walter L. Robb Chair Professor of Chemical Engineering Head of the Department of Chemical Engineering *Signatures are on file in the Graduate School iii ABSTRACT Polymer nanofibers are 1D nanostructures that are gathering significant interest because of their potential applications in a wide variety of fields such as biomedicine, separation, electronics and sensor materials. They are also fascinating structures because in some cases they posses unique properties arising from the preferential arrangement of the polymer chains parallel to the fibers axes. Challenges that synthesis techniques for polymer nanofibers face are scalability and control during fabrication. An alternate to current common approaches such as electrospinning and templated-synthesis of polymer nanofibers, is template-less synthesis of polymer nanofibers during polymerization. This approach offers the advantage of bottom-up fabrication and the potential for large scale synthesis. Herein results from an investigation using this approach for poly (ethyl 2- cyanoacrylate) [PECA] nanofiber formation are reported. The template-less growth of PECA nanofibers is first demonstrated using the initiators present in human fingerprint residue via vapor phase polymerization of the monomer under conditions of high humidity. Studies showed that anionic initiators like the Cl - ion present in fingerprint residues is responsible for fiber formation whereas other anions such as OH - results in the formation of a polymer film under the same conditions of polymerization. Insights into individual initiator effects reveal a classification of the initiators to explain the basis for the morphology of the polymer obtained (1D fiber or 2D film). The classification based on the Hard Soft Acid Base principle implies that for faster initiation (achieved by harder anions) a polymer film is obtained versus polymer nanofibers that are obtained for slower initiation (achieved by softer anions). This iv suggests that for faster initiation two dimensional growth of the polymer occurs versus one dimensional growth for slower initiation rates leading to fiber formation. This technique is also extended to demonstrate growth of PECA nanofibers on silane-modified glass slides with varying fiber densities depending upon ECA (monomer) wettability of the glass surface. These results showcase the ability of control over placement of the fibers using this template-less synthesis approach. Finally two examples of exercising control during synthesis of polymer nanofibers are provided. In the first case by controlling conditions during polymerization, termination steps are varied to create polymer nanofibers with different molecular weights. In the second case, random copolymer nanofibers of ethyl 2-cyanoacrylate and methyl 2-cyanoacrylate are formed by introducing both monomers simultaneously during nanofiber synthesis. v TABLE OF CONTENTS LIST OF FIGURES .....................................................................................................ix LIST OF TABLES.......................................................................................................xiv ACKNOWLEDGEMENTS.........................................................................................xv Chapter 1 Introduction and Background for Polymer Nanofibers..............................1 1.1 Interest in 1D Nanostructures .........................................................................1 1.2 Why Polymer Nanofibers? .............................................................................3 1.2.1 Application of Polymer Nanofibers......................................................5 1.2.2 Unique properties of Polymer Nanofibers............................................8 1.3 Synthesis techniques for Polymer Nanofibers................................................9 1.3.1 Electrospinning of Polymer Nanofibers ...............................................9 1.3.1.1 Details of electrospinning process..............................................10 1.3.1.2 Capabilities of electrospinning process......................................11 1.3.2 Templated synthesis of Polymer Nanofibers........................................13 1.3.2.1 Mesoporous channel templates ..................................................14 1.3.2.2 Porous membranes as templates.................................................15 1.3.3 Template-less techniques for creating Polymer Nanofibers.................17 1.4 Motivation and Goals of this work .................................................................19 1.5 Background information on Ethyl 2-cyanoacrylate........................................20 1.5.1 Polymerization of ECA ........................................................................21 1.5.2 Uses of cyanoacrylates .........................................................................23 1.6 Organization of the Thesis..............................................................................25 1.7 References.......................................................................................................26 Chapter 2 Experimental Section; Methods and Materials ..........................................29 2.1 Techniques for Polymer Synthesis .................................................................29 2.1.1 Batch Set-up for Polymerization ..........................................................29 2.1.2 Semi-continuous Flow Set-up for Polymerization ...............................32 2.2 Techniques for Applying Initiators on Substrates ..........................................34 2.2.1 Spin-coating initiator solutions.............................................................35 2.2.2 Silanation..............................................................................................35 2.3 Characterization Techniques ..........................................................................36 2.3.1 Scanning Electron Microscopy (SEM).................................................36 2.3.2 Infra-red Spectroscopy (IR)..................................................................37 2.3.3 Gel Permeation Chromatography (GPC)..............................................38 2.3.4 X-ray Photoelectron Spectroscopy (XPS)............................................39 2.3.5 Atomic Force Microscopy (AFM)........................................................39 2.4 Materials .........................................................................................................40 vi 2.5 References.......................................................................................................41 Chapter 3 Template-less Growth of Poly(ethyl 2-cyanoacrylate) Nanofibers by Initiators Present in Fingerprints ..........................................................................42 3.1 Introduction.....................................................................................................42 3.2 Experimental Section......................................................................................43 3.2.1 Materials...............................................................................................43 3.2.2 Methods ................................................................................................44 3.3 Results.............................................................................................................44 3.3.1 Fingerprint fuming................................................................................44 3.3.2 Investigation of fingerprint residue components for PECA nanofiber formation................................................................................48 3.4 Discussion.......................................................................................................54 3.4.1 Formation of nanofibers .......................................................................54 3.4.2 Initiators for nanofiber formation.........................................................56 3.5 Conclusions.....................................................................................................57 3.6 References.......................................................................................................57 Chapter 4 Influence of Initiators on the Growth of Poly (ethyl 2-cyanoacrylate) Nanofibers.............................................................................................................59 4.1 Introduction.....................................................................................................59 4.2 Experimental Section......................................................................................60 4.2.1 Materials...............................................................................................60 4.2.2 Methods ................................................................................................60 4.3 Results and Discussion ...................................................................................61
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