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Modification of Paper Into Conductive Substrate for Electronic Functions Faculty of Technology and Science Chemical Engineering Elson Montibon Modification of Paper into Conductive Substrate for Electronic Functions Deposition, Characterization and Demonstration DISSERTATION Karlstad University Studies 2010:28 Elson Montibon Modification of Paper into Conductive Substrate for Electronic Functions Deposition, Characterization and Demonstration Karlstad University Studies 2010:28 Elson Montibon. Modification of Paper into Conductive Substrate for Electronic Functions - Deposition, Characterization and Demonstration Dissertation Karlstad University Studies 2010:28 ISSN 1403-8099 ISBN 978-91-7063-361-4 © The Author Distribution: Karlstad University Faculty of Technology and Science Chemical Engineering S-651 88 Karlstad Sweden +45 54 700 100 www.kau.se Print: Universitetstryckeriet, Karlstad 2011 “Delight thyself also in the LORD: and he shall give thee the desires of thine heart.” Psalm 37:4 Abstract The thesis investigates the modification of paper into an ion- and electron-conductive material, and as a renewable material for electronic devices. The study stretches from investigating the interaction between cellulosic materials and a conducting polymer to demonstrating the performance of the conductive paper by printing an electronic structure on the surface of the conductive paper. Conducting materials such as conducting polymer, ionic liquids, and multi-wall carbon nanotubes were deposited into the fiber networks. In order to investigate the interaction between the conducting polymer and cellulosic material, the adsorption of the conducting polymer poly(3,4-ethylenedioxythiophene): poly(4-styrene sulfonate) (PEDOT:PSS) onto microcrystalline cellulose (MCC) was performed. The adsorption isotherm showed a broad molecular distribution of the conducting polymer and considerable interaction between the polymer and the MCC. The amount adsorbed decreased with increasing pH of the dispersion and varying the salt concentration of the solution revealed that the adsorption passed through a maximum. Papers displaying electroconductive behavior were produced via dip coating and rod coating, and characterized. The Scanning Electron Microscopy (SEM) / Energy Dispersive Spectroscopy (EDS) images showed that the conducting polymer was deposited in the fiber and in fiber-fiber contact areas. The X-ray Photoelectron Spectroscopy (XPS) analysis of dip-coated paper samples showed PEDOT enrichment on the surface. The degree of washing of the dip-coated paper with dilute acid did not significantly affect the PEDOT enrichment on the surface. When the base paper was coated with a PEDOT:PSS blend, the conductivity increased by many orders of magnitude. The base papers normally had bulk conductivities in the region of 10 -12 S/cm, and after modification, the conductivity reached between 10 -3 and 10 -1 S/cm. The effects of fiber beating and paper formation were also investigated. The presence of organic solvents N-methyl-2-pyrrolidone (NMP) and dimethyl sulfoxide (DMSO) in the PEDOT:PSS dispersion enhanced the conductivity of the coated sheets, while sorbitol and isopropanol had no enhancement effect. This is due to the conformational changes of the PEDOT molecule in the presence of NMP and DMSO and to their plasticizing effect. The conductivity of paper did not increase until the line load reached 174 kN/m during calendering which is indicative of PEDOT:PSS being suspended in the fiber network. The effect of the presence of pigments such as titanium dioxide (TiO 2) and multi-wall carbon nanotubes (MWCNT) was also discussed, and also their effects on other properties such as tensile strength, surface property and wetting were discussed. i Ionic paper was produced by depositing an ionic liquid into the commercial base paper. The effect of humidity on the ionic conductivity was determined. Even at a humidity as low as 25% RH, the ionic paper demonstrated good ionic conductivity. The temperature- dependence of the ionic conductivity followed the simple Arrhenius equation, which can be attributed to the hopping of carrier ions. The ionic paper was surface-sized in order to reduce the roughness and improve its printability. The bulk resistance increased with increasing surface sizing. The electrochemical performance of the ionic paper was confirmed by printing PEDOT:PSS on the surface. There was change in color of the polymer when a voltage was applied. It was demonstrated that the ionic paper is a good ionic conductor that can be used as a component for a more compact electronic device construction. Conductive paper has a great potential to be a flexible platform on which an electronic structure can be constructed. The conduction process in the modified paper is due to the density of charge carriers (ions and electrons), and their short range mobility in the material. The charge carrying is believed to be heterogeneous, involving many species as the paper material is chemically heterogeneous. Paper is a versatile material. Its bulk and surface properties can easily be tuned to a desired level by modifying the fibers, adding chemical additives, and surface treatment. Furthermore, the abundance of cellulosic material on this planet makes conductive paper a renewable and sustainable component for electronic devices. ii List of Papers I Characterization of Poly(3,4.ethylenedioxythiophene):Poly(4-styrenesulfonate) (PEDOT:PSS) on Cellulosic Materials Elson Montibon, Lars Järnström, and Magnus Lestelius Cellulose 2009 , 16, 807-815 II Electroconductive Paper Prepared by Coating with Blends of Poly(3,4- ethylenedioxythiophene)/Poly(4-styrenesulfonate) (PEDOT:PSS) and Organic Solvents Elson Montibon, Magnus Lestelius, and Lars Järnström Journal of Applied Polymer Science 2010 , 117, 3524-3532 III. Electroconductive Paper – a study of conductivity achieved through polymer deposition and papermaking properties Elson Montibon, Karen T. Love, Magnus Lestelius, and Lars Järnström Nordic Pulp and Paper Research Journal 2010 , 25 (4), 473-480 IV Conductivity of paper containing poly(3,4-ethylenedioxythiophene)/poly(4- styrenesulfonate) and multi-wall carbon nanotubes Elson Montibon, Magnus Lestelius, and Lars Järnström Submitted for publication in Journal of Applied Polymer Science V Porous and Flexible Ionic Paper as a platform for compact electronic devices Elson Montibon, Magnus Lestelius and Lars Järnström Manuscript to be submitted for publication Reprints of Papers I, II, and III have been made with permission from the publishers Elson Montibon’s contribution to the papers Elson Montibon performed all the experimental work with the exception of XPS in Paper I; BET area in Papers I and II; SEM/EDS in Papers II, III and IV; and Hg-porosimetry in Paper III. Elson is the main author of all five papers included in this thesis. iii Related presentations by the same author Montibon E., Järnström L., and Lestelius M., “On Investigation of Poly(3,4.ethylenedioxythiophene)/Poly(4-styrenesulfonate) (PEDOT:PSS) Adsorption on Cellulosic Materials”, Poster Presentation, Conference Proceeding of the Nordic Polymer Days 2008, Stockholm, Sweden, June 11-13, 2008. Montibon E., Järnström L., and Lestelius M., “Characterization of Poly(3,4- ethylenedioxythiophene)/Poly(4-styrenesulfonate) (PEDOT:PSS) Adsorption on Cellulosic Materials”, Oral Presentation, Conference Proceeding of 13th IACIS International Conference on Surface and Colloid Science, and the 83rd ACS Colloid & Surface Science Symposium, Columbia University, New York City, USA. June 14-19, 2009. Montibon E., Lestelius M., and Järnström L. “Preparation of Electroconductive Paper by Coating Blends of Poly(3,4-ethylenedioxythiophene)/Poly(4-styrenesulfonate) (PEDOT:PSS) and Organic Solvents,” Oral Presentation, Proceedings of the TAPPI Coating and Graphic Arts Conference (PaperCon ‘09), St. Louis, Missouri, USA, May 31 – June 03, 2009. Lestelius M., Montibon E., and Järnström L. “Preparation of Electroconductive Paper by Deposition of Conducting Polymer,” Oral Presentation, Innovative Packaging Symposium, PTS, Munich, Germany, June 05-06, 2010. Montibon E., Lestelius M., and Järnström L. “Modification of Paper into Electroconductive Material by Deposition of Conducting Polymer Blends”, Oral Presentation, Proceedings of the 3 rd International Symposium of Emerging Technologies in Pulping and Papermaking (ISETPP ), SCUT, Guangzhou, China, November 8-10, 2010. iv List of Symbols and Abbreviations Abbreviations AU - absorbance unit BSE - Backscattered electron CD - cross machine direction CNT - carbon nanotubes DMSO - Dimethyl sulfoxide EDS - Energy Dispersive X-ray Spectroscopy ESCA - Electron Spectroscopy for Chemical Analysis FFT - fast Fourier transform HOMO - highest occupied molecular orbital IS - impedance spectroscopy LUMO - lowest unoccupied molecular orbital IL - ionic liquid MCC - microcrystalline cellulose MD - machine direction MWCNT - multi-wall carbon nanotubes NMP - N-methyl-2-pyrrolidone PEDOT:PSS - poly(3,4-ethylenedioxythiophene)/poly(4-styrene sulfonate) PSI - phase shift interferometer RBA - relative bonded area RTIL - room temperature ionic liquid SWCNT - single wall carbon nanotubes VSI - vertical scanning interferometer XPS - X-ray Photoelectron spectroscopy Symbols a - cross-section area (m 2) A - measured absorbance (AU) E - applied electric field (N/C) E1 - heat of adsorption of layer 1 (J) EL - heat of adsorption of higher layers (J) Ea - activation energy (eV or J) Eb - binding energy (eV or J) Ek - kinetic energy (eV or J) e - elementary charge (1.602176487 x 10 -19
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