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a wide range of conductivity in these conductive porous devices. It also opens up the potential to develop these devices as load bearing sensors. 5.5 Conclusions This paper reports on the preparation of a novel 3D porous polymeric conducting device (PPCD) derived from multi-percolated polymer blend systems. The work has focused on the preparation of ultra low surface area porous substrates followed by the deposition of polyaniline conductive polymer (PANI) on the internal porous surface using a layer-by-layer technique. In this way, the percolation threshold of PANI in this porous conductive device can be reduced to a value as low as 0.19%. Furthermore, depending on the amount of PANI deposited, the electrical conductivity of the porous substrate can be controlled over several orders of magnitude from 10 -15 S cm -1 to 10 -3 S cm -1 . Ternary and quaternary multi-percolated(hierarchically ordered) systems comprised of highdensity polyethylene (HDPE), polystyrene (PS), poly(methyl methacrylate) (PMMA) and poly(vinylidene fluoride) (PVDF) are melt-mixed and subsequently annealed in order to obtain large interconnected phases. Subsequent extraction of PS, PMMA and PVDF within that blend allows for the preparation of a fully interconnected porous HDPE substrate of ultra-low surface area and highly uniform sized channels. This provides an ideal substrate for subsequent polyaniline (PANI) addition. Using a layer-by-layer (LbL) approach, alternating poly(styrene sulfonate) (PSS)/PANI layers are deposited on the internal surface of the 3-dimensional porous polymer substrate. The PANI and sodium poly(styrene sulfonate) (NaPSS) both adopt an interdiffused network conformation on the surface. The sequential mass deposition of PSS and PANI multilayers has been studied in detail and an oscillating behavior is observed, due primarily to the diffusion of PSS chains both in and out of the multilayer structure. Salt in the deposition solution highly affects the polyelectrolyte construction by allowing for a more uniform deposition and more thickly deposited PSS/PANI layers. The mass deposition growth for the PSS/PANI system in all cases is not linear. Conductivity measurements show that the conductivity of these samples increases from 10 -15 S cm -1 to 10 -5 S cm -1 as the number of 168
deposited PANI layers increases until a saturation plateau is reached at approximately 32 layers. The conductive porous polymer device developed in this study is sensitive to applied compression providing that the void volume percentage is sufficiently high. Higher loads result in higher conductivity values with values as high as 10 -3 S cm -1 obtained. Although this approach has been demonstrated here for an ultra-low surface area porous substrate, high surface area substrates can also be readily prepared. 5.6 Acknowledgements The authors express appreciation to the Natural Sciences and Engineering Research Council of Canada for supporting this work. They also thank F. Normandin from the Institut des matériaux industriels for his assistance with the conductivity measurements of the samples. 5.7 References (1) Heywang, G.; Jonas, F. Advanced Materials 1992, 4, 116. (2) Roman, L. S.; Andersson, M. R.; Yohannes, T.; Inganás, O. Advanced Materials 1997, 9, 1164. (3) Kraft, A.; Grimsdale, Andrew C.; Holmes, Andrew B. Angewandte Chemie 1998, 110, 416. (4) Schmidt, V. M.; Tegtmeyer, D.; Heitbaum, J. Journal of Electroanalytical Chemistry 1995, 385, 149. (5) Wessling, B. Advanced Materials 1994, 6, 226. (6) Contractor, A. Q.; Sureshkumar, T. N.; Narayanan, R.; Sukeerthi, S.; Lal, R.; Srinivasa, R. S. Electrochimica Acta 1994, 39, 1321. (7) Kaneto, K.; Kaneko, M.; Min, Y.; MacDiarmid, A. G. Synthetic Metals 1995, 71, 2211. (8) Burroughes, J. H.; Bradley, D. D. C.; Brown, A. R.; Marks, R. N.; Mackay, K.; Friend, R. H.; Burns, P. L.; Holmes, A. B. Nature 1990, 347, 539. (9) Margolis, J. M. Conductive Polymers and Plastics; Chapman and Hall: New York, 1989. (10) Halls, J. J. M.; Walsh, C. A.; Greenham, N. C.; Marseglia, E. A.; Friend, R. H.; Moratti, S. C.; Holmes, A. B. Nature 1995, 376, 498. (11) Tessler, N.; Denton, G. J.; Friend, R. H. Nature 1996, 382, 695. (12) Garnier, F.; Hajlaoui, R.; Yassar, A.; Srivastava, P. Science 1994, 265, 1684. (13) Zasadzinski, J. A.; Viswanathan, R.; Madsen, L.; Garnaes, J.; Schwartz, D. K. Science 1994, 263, 1726. (14) Maoz, R.; Frydman, E.; Cohen, S. R.; Sagiv, J. Advanced Materials 2000, 12, 424. 169
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© Sepehr Ravati, 2010. UNIVERSITÉ
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DEDICATED To my parents iii
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RÉSUMÉ Cette thèse présente, po
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devenir une structure hiérarchique
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ABSTRACT This thesis presents, for
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system can be increased from 10 -15
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CONDENSÉ EN FRANÇAIS Dans ce trav
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deuxième coquille de PS. Les phase
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structures à percolation multiple
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autre sous-type de morphologie dans
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TABLE OF CONTENTS DEDICATION.......
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xxiii 2.4.1.1.1 Charged Polymer Ads
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5.3.4 Annealing Test ..............
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xxvii REFERENCES ..................
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LIST OF FIGURES xxix Figure 1-1. a)
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Figure 2-12. SEM photomicrograph of
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Figure 2-34. Schematic view of diff
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Figure 4-8. SEM micrographs of vari
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Figure 5-6. a),b) Scanning electron
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and c) triangular concentration dia
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n number of moles p concentration o
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AFM atomic force microscopy LIST OF
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PS-co-PMMA copolymer of PS and PMMA
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1.1 Introduction CHAPTER 1 - INTROD
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Figure 1-2. Human heart, longitudin
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One of the applications for porous
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On the other hand, a novel tri-cont
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2.1 Polymer Blends CHAPTER 2 - LITE
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Based on Sterling’s approximation
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Antonoff’s rule (Equation 2-13) i
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2.1.2.1 Binary Polymer Blends 2.1.2
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Some other studies(Everaert, Aerts,
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where the parameter z is dependent
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“compatibilization” was suggest
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a) λ BC A and B are matrices, b) C
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Reignier & Favis, 2000, 2003a; Reig
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measure the interfacial tension of
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a) b) Figure 2-6. Dependence of the
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Omonov et al. found double percolat
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2.1.2.2.3 Effect of Composition on
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a) b) C B A c) Figure 2-12. SEM pho
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In the case where PS is the matrix,
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Posthuma de Boer, 1999) (Kumin & Ch
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lattice, such as square lattice, wi
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magnetization, which is a function
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Polymers have long been thought of
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epoxy as a function of nanotube wei
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Figure 2-19. Approaching the percol
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Figure 2-21. Transmission electron
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Figure 2-22: Dependence of PE conti
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Figure 2-24. Plot of the total numb
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chain provides the conductive path
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2.3.1.2.1 Polyaniline One of the mo
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CoPA/LLDPE/PANI blend and a poor-qu
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Narkis and co-workers extended and
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Figure 2-31: Conductivity of PVDF/P
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organic thin films, a novel and str
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on the topic have been reported in
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succeeded in creating thin films wi
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Addition of salt to the solution of
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different from that of linear homop
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Figure 2-39. Macromolecule with a)
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polyanion such as hyaluronan (HA)(P
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2.4.1.1.7 Effect of Salt on Multila
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2.4.1.1.8 Overcompensation of the M
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important factors determining the g
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As shown in Figure 2-44, swelling a
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increasing the pH value due to a de
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CHAPTER 3 - ORGANIZATION OF THE ART
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discussed above, HDPE, PS, PMMA, an
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CHAPTER 4 - LOW PERCOLATION THRESHO
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or model which predicts where the p
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concentration threshold for the ons
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chemical and weathering resistance,
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Table 4-1. Material Characteristics
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filled with blend pellets. To facil
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4.3.6 Conductivity Measurements DC
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experimentally in this research gro
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a) b) c) d) Figure 4-4. Schematic i
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microstructure of the quaternary bl
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a) b) c) d) Figure 4-6. SEM microgr
Page 163 and 164: a) b) PVDF PS PMMA c) d) e) HDPE PS
Page 165 and 166: Uniform layers of PS and PMMA situa
Page 167 and 168: the concentration of HDPE is increa
Page 169 and 170: a) b) c) e) Figure 4-11. SEM microg
Page 171 and 172: melt-processable and contains 25 wt
Page 173 and 174: One question that should be address
Page 175 and 176: Conductivity(S/cm) Ternary Blend 1,
Page 177 and 178: phase(PMMA), the concentration of P
Page 179 and 180: (6) Virgilio, N.; Desjardins, P.; L
Page 181 and 182: ONION MORPHOLOGY HDPE PVDF PS Contr
Page 183 and 184: work described above has focused on
Page 185 and 186: thermodynamic explanation to predic
Page 187 and 188: four-point probe increases continuo
Page 189 and 190: in the rheology tests were compress
Page 191 and 192: 5.3.6 Layer-by-Layer Deposition The
Page 193 and 194: prepare a polymer blend structure w
Page 195 and 196: a) b) c) Figure 5-3. Scanning elect
Page 197 and 198: spontaneously self-assembled. After
Page 199 and 200: a) b) c) d) e) f) g) h) Figure 5-5.
Page 201 and 202: Since the ultra-low surface area va
Page 203 and 204: c) a) b) Figure 5-6. a),b) Scanning
Page 205 and 206: salt to a PSS polyelectrolyte solut
Page 207 and 208: A relationship between macropore si
Page 209 and 210: close together. It is interesting t
Page 211 and 212: Figure 5-9. Mass increase (%) indic
Page 213: In this work the conductance of the
Page 217 and 218: (52) Guo, H. F.; Packirisamy, S.; G
Page 219 and 220: 6.2 Introduction It is well-known t
Page 221 and 222: modified version of Harkins theory(
Page 223 and 224: 6.3 Experimental 6.3.1 Materials Co
Page 225 and 226: Complex voscosity (Pa.s) 1,0E+04 1,
Page 227 and 228: 6.3.5.2 Focused Ion Beam (FIB) and
Page 229 and 230: a) c) b) d) e) f) PMMA PMMA HDPE HD
Page 231 and 232: y Harkins theory, PS will always si
Page 233 and 234: a) b) c) d) e) f) PS Figure 6-6. a)
Page 235 and 236: a) b) HDPE : black PS : grey PMMA :
Page 237 and 238: 6.4.6 Continuity, Co-continuity, an
Page 239 and 240: c) V III II I VII I IV VI Figure 6-
Page 241 and 242: Continuity Scheme (a) Figure 6-10.
Page 243 and 244: Addition of a low concentration of
Page 245 and 246: Addition of small amounts of HDPE t
Page 247 and 248: icontinuous network with the HDPE.
Page 249 and 250: Three examples are shown in Figure
Page 251 and 252: (9) Mekhilef, N.; Verhoogt, H. Poly
Page 253 and 254: structures are formed due to the co
Page 255 and 256: CONCLUSION AND RECOMMENDATIONS In t
Page 257 and 258: REFERENCES A. K. Gupta, K. R. S. (1
Page 259 and 260: Caruso, F. (2003). Hollow Inorganic
Page 261 and 262: Domenech, S. C., Bortoluzzi, J. H.,
Page 263 and 264: Geuskens, G., Gielens, J. L., Geshe
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Hou, S., Harrell, C. C., Trofin, L.
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Krass, H., Papastavrou, G., & Kurth
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Macdiarmid, A. G., Jin-Chih, C., Ha
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Niziol, J., & Laska, J. (1999). Con
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Reghu, M., Yoon, C. O., Yang, C. Y.
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Shirakawa, H., Louis, E. L., MacDia
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Utracki, L. A. (1991). On the visco
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Yasuda, K., Armstrong, R., & Cohen,
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literature has examined factors inf
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(Reignier & Favis, 2000, 2003a; Rei
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Table A-1.2. Interfacial tensions a
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acquisition of images with a very h
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Table A-1.3. Continuity of the PMMA
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(17) Reignier, J.; Favis, B. D., Ma
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PANI. Theoretically, the extent of
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Equation A-2.7 0( ) 0 1. 5 σ = σ
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Cumulative Mass × 10 5 (g) dipping
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of PANI, and an increase in the con
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Resistance(ohm) 1.0E+12 1.0E+11 1.0
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esistance value. Samples containing
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The results of resistance for PS/PE
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Caruso, F., & Schuler, C. (2000). E
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