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5.4.3 Continuity and Surface Areas of Substrates Table 5-3 shows gravimetric data obtained after solvent extraction and demonstrates that in all cases the various phases within the HDPE are fully continuous. The continuity of all extracted phases for both annealed and unannealed samples is higher than 96%. Hence, the 33% volume fraction of HDPE in samples A and B and 40% in samples C and D results in a 67% and 60% void volume respectively after the extraction of all other phases. As well, the effect of annealing on reducing the surface area of the porous substrate is extremely evident as it was below the range which could be measured quantitatively by BET (Table 5-4). Table 5-3. Continuity of the Porous Morphology With and Without annealing (PS, PMMA and PVDF extracted). Sample Continuity of (PS+PMMA+PVDF) no annealing Continuity of (PS+PMMA+PVDF) with annealing A 96.6 % 98.3 % B 98 % 100 % C 98.3 % 99.3 % D 96 % 97.4 % Table 5-4. Surface Area Measurements of Porous Polymer Substrates by BET Sample Surface area measured by BET(m2 /g) no annealing Surface area measured by BET(m 2 /g) with annealing A 1.28 < 0.01 B 0.70 < 0.01 C 0.88 < 0.01 D 0.74 < 0.01 154
Since the ultra-low surface area values are beyond the range of the BET equipment, the surface area of sample A (morphology shown in Figure 5-5e) was estimated arithmetically. A porous disc-shape sample with a diameter of 2.5-cm and a length of 1-mm is assumed to be comprised of numerous parallel cylinders from top to bottom with a diameter of 175-µm and a length of 1mm. The diameter of cylinders is obtained from average diameter of HDPE cylindrical rods exhibited in Figure 5-5e. Estimating the number of cylinders and the surface area per cylinder as 6818 and 0.00375m 2 /g, respectively, corresponds to a surface area of the porous device of approximately 0.01 m 2 /g. Hence, the work to this point has achieved fully interconnected porous substrates (samples A, B, C, and D) of ultra-low surface area (large pores) and a highly uniform pore size. All these samples will be used as substrates for the layer-by-layer deposition of polyaniline in the subsequent parts of this work. Table 5-5 compares the surface area of porous sample A to the surface area of other co-continuous systems and demonstrates that, to our knowledge, this is the lowest surface area, fully interconnected porous polymer material ever presented in the literature. Table 5 also demonstrates the potential of preparing conductive devices from higher surface area co-continuous systems and underlines the versatility of the approach. 155
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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,
Page 149 and 150: Table 4-1. Material Characteristics
Page 151 and 152: filled with blend pellets. To facil
Page 153 and 154: 4.3.6 Conductivity Measurements DC
Page 155 and 156: experimentally in this research gro
Page 157 and 158: a) b) c) d) Figure 4-4. Schematic i
Page 159 and 160: microstructure of the quaternary bl
Page 161 and 162: 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: a) b) c) d) e) f) g) h) Figure 5-5.
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 and 214: In this work the conductance of the
Page 215 and 216: deposited PANI layers increases unt
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
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(9) Mekhilef, N.; Verhoogt, H. Poly
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structures are formed due to the co
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CONCLUSION AND RECOMMENDATIONS In t
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REFERENCES A. K. Gupta, K. R. S. (1
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Caruso, F. (2003). Hollow Inorganic
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Domenech, S. C., Bortoluzzi, J. H.,
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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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