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continuous structure of PEMA and HDPE with larger phase sizes. Therefore, a large part of the blend is occupied by thick rods of HDPE. Since the PEMA phase, located at the interface, makes some connected pathways, and PANI is distributed in the PEMA, in this case geometrical restriction results in producing a few connected pathways of PANI in 30% PEMA. Because of the constitution of small clusters of PANI in the PEMA intermediate phase, the resistance slightly decreases. Increasing further the amount of PEMA results in a tri-continuous morphology for 45/45/10 HDPE/PEMA/PANI, since with a sufficient content of PEMA, a continuous phase of PEMA forms and consequently the small amount of PANI phase inside it becomes continuous. As the continuous HDPE phase still occupies 45% of the blend, and due to the formation of larger connected pathways of PANI, resistance reduces by almost three orders of magnitude. Addition of further PEMA to the blend results in a preparation of 30/60/10 in which the continuous structure of HDPE starts to convert to droplets. Due to the lower occupation of space with HDPE, and the dispersion of PANI in a higher amount of PEMA, 10% PANI distributes as droplets and connected pathways are hardly constructed. Increasing the concentration of PEMA to 10/80/10 HDPE/PEMA/PANI results in the formation of bicontinuous/droplet morphology, whereas a small content of HDPE causes a vast occupation area of PEMA. Therefore, 10% PANI particles disperse in PEMA, showing a higher value of resistance. Finally, for a binary blend of 90/10 PEMA/PANI, matrix/droplet morphology is predicted, although still one or two connected pathway of PANI in PEMA can be found. As it is observed, concentration and morphology of HDPE and PEMA affect the conductivity and continuity of PANI, where the percolation threshold of samples with a constant 10% of PANI is obtained at 35% of PEMA and 90% of PEMA in a HDPE/PEMA/PANI ternary blend. In samples containing 20% of PANI, a similar behavior for small contents of PEMA with a slight difference in the value of resistance is observed. At 40/40/20 HDPE/PEMA/PANI, tri-continuous morphology is generated, demonstrating a sharp decrease of the resistance. The important points are samples containing 20% PANI and 66.6/33.3 PEMA/HDPE and 90/10 PEMA/HDPE in which, in contrast to samples containing 10% of PANI at these points, resistance has a low value. As mentioned above, higher value of resistance at these points for samples containing 10% of PANI is related to droplets of PANI distributed in PEMA, due to lack an insufficient amount of PANI. On the contrary, for samples containing 20% of PANI, the concentration of PANI is high enough to form a number of connected pathways of PANI inside PEMA, yielding the decrease of 256
esistance value. Samples containing 30% of PANI, because of the high amount of PANI in the sample, reveal high values of conductivity for a wide range of concentrations. Only in the first region of the curve (high concentration of HDPE), due to the presence of a large volume fraction of HDPE, is the value of conductivity low. The percolation threshold occurs at 10% of PEMA, as a double-percolated morphology is predicted for this ternary blend containing of 60/10/30 HDPE/PEMA/PANI. By increasing the amount of PEMA, the morphology tends to become tri- continuous, since the network of PANI contributes throughout the entire sample. The second ternary blend, comprised of PS/PEMA/PANI, was chosen with the same compositions of components. Since the interfacial tension between PS and PEMA (γPEMA/PS = 1.3 mN/m) is much lower than that for HDPE and PEMA (γPEMA/HDPE = 8.3 mN/m), it is predicted that PS and PEMA will make smaller phase sizes than HDPE and PEMA. Although it is difficult to show the morphological features of a ternary PS/PEMA/PANI blend, the decrease of the phase sizes between PS and PEMA are shown in the HDPE/PS/PANI blend. Figure A-4.4 shows the morphology of an interdiffusion of PEMA and PS in the HDPE/PS/PANI blend, representing very small rods and branches of PEMA after extraction of PS, while the rods of the continuous phase of HDPE are so large. Such differences in the sizes of trunks of continuous HDPE and PEMA indicate how much the interfacial tension differs between PEMA and either of these two phases. 257
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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
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a) b) PVDF PS PMMA c) d) e) HDPE PS
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Uniform layers of PS and PMMA situa
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the concentration of HDPE is increa
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a) b) c) e) Figure 4-11. SEM microg
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melt-processable and contains 25 wt
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One question that should be address
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Conductivity(S/cm) Ternary Blend 1,
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phase(PMMA), the concentration of P
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(6) Virgilio, N.; Desjardins, P.; L
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ONION MORPHOLOGY HDPE PVDF PS Contr
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work described above has focused on
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thermodynamic explanation to predic
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four-point probe increases continuo
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in the rheology tests were compress
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5.3.6 Layer-by-Layer Deposition The
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prepare a polymer blend structure w
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a) b) c) Figure 5-3. Scanning elect
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spontaneously self-assembled. After
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a) b) c) d) e) f) g) h) Figure 5-5.
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Since the ultra-low surface area va
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c) a) b) Figure 5-6. a),b) Scanning
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salt to a PSS polyelectrolyte solut
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A relationship between macropore si
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close together. It is interesting t
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Figure 5-9. Mass increase (%) indic
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In this work the conductance of the
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deposited PANI layers increases unt
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(52) Guo, H. F.; Packirisamy, S.; G
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6.2 Introduction It is well-known t
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modified version of Harkins theory(
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6.3 Experimental 6.3.1 Materials Co
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Complex voscosity (Pa.s) 1,0E+04 1,
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6.3.5.2 Focused Ion Beam (FIB) and
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a) c) b) d) e) f) PMMA PMMA HDPE HD
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y Harkins theory, PS will always si
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a) b) c) d) e) f) PS Figure 6-6. a)
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a) b) HDPE : black PS : grey PMMA :
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6.4.6 Continuity, Co-continuity, an
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c) V III II I VII I IV VI Figure 6-
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Continuity Scheme (a) Figure 6-10.
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Addition of a low concentration of
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Addition of small amounts of HDPE t
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icontinuous network with the HDPE.
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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
Page 265 and 266: Hou, S., Harrell, C. C., Trofin, L.
Page 267 and 268: Krass, H., Papastavrou, G., & Kurth
Page 269 and 270: Macdiarmid, A. G., Jin-Chih, C., Ha
Page 271 and 272: Niziol, J., & Laska, J. (1999). Con
Page 273 and 274: Reghu, M., Yoon, C. O., Yang, C. Y.
Page 275 and 276: Shirakawa, H., Louis, E. L., MacDia
Page 277 and 278: Utracki, L. A. (1991). On the visco
Page 279 and 280: Yasuda, K., Armstrong, R., & Cohen,
Page 281 and 282: literature has examined factors inf
Page 283 and 284: (Reignier & Favis, 2000, 2003a; Rei
Page 285 and 286: Table A-1.2. Interfacial tensions a
Page 287 and 288: acquisition of images with a very h
Page 289 and 290: Table A-1.3. Continuity of the PMMA
Page 291 and 292: (17) Reignier, J.; Favis, B. D., Ma
Page 293 and 294: PANI. Theoretically, the extent of
Page 295 and 296: Equation A-2.7 0( ) 0 1. 5 σ = σ
Page 297 and 298: Cumulative Mass × 10 5 (g) dipping
Page 299 and 300: of PANI, and an increase in the con
Page 301: Resistance(ohm) 1.0E+12 1.0E+11 1.0
Page 305 and 306: The results of resistance for PS/PE
Page 307 and 308: Caruso, F., & Schuler, C. (2000). E
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