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A-1.2. Experimental Section A-1.2.1. Materials: HDPE 04352N and PS 615APR were both obtained from the Dow Chemical Company. PMMA 200336 was purchased from Sigma-Aldrich. An antioxidant, Irganox B225 from Ciba-Geigy, was added to the mixture to reduce thermal oxidation of polyethylene (0.2 weight percent). Physical properties of the materials were measured previously (Reignier & Favis, 2003a) and are given in Table A-1.1. Table A-1.1. Homopolymer properties Polymers M w a ×10- 3 g/mol M n a ×10-3 g/mol Melt Index b ASTM g/10min Density b g/cm3 at 20°C 200°C η 1* × 10-3 c Pa.s at 200°C N 1 × 10-4 d Pa at 200°C HDPE 79 24 4 0.96 0.75 1.2 1.2 2.2 2.2 PS 290 141 15 1.04 0.97 1.7 2.6 11 5.1 PMMA 11.9 7.8 - - 1 0.04 0.04 0.02 0.6 a Measured by GPC, b Obtained from supplier, c η * is the complex viscosity, d N1 is the first normal stress difference, e At average shear rate during blending: 1 25 − • γ = s , f 4 At average shear stress during blending: τ = 2 . 7× 10 Pa A-1.2.1. Measurement of the interfacial tensions and calculation of the spreading coefficients: The interfacial tensions were measured using the breaking thread method, as described in an earlier publication (Reignier & Favis, 2000). The different interfacial tensions and spreading coefficients for the HDPE/PS/PMMA ternary blends are given in Table A-1.2. γ& e f τ γ& τ 238
Table A-1.2. Interfacial tensions and spreading coefficients for HDPE/PS/PMMA blends at 200°C. Polymer pairs % Interfacial tension Continuity γ (mN/m) m = m initial − m ( i ) initial final × Polymer pairs Spreading of i on j (i/j) 100 Spreading coefficients λ (mN/m) HDPE/PS 5.1 PS/PMMA 1.1 PS/PMMA 2.4 PMMA/PS -5.9 HDPE/PMMA 8.6 HDPE/PS -11.3 A-1.2.3. Blend preparation: Prior to melt mixing, all polymers were pre-dried for 24h at 80°C in a vacuum oven to remove any moisture from the pellets or powders. Ternary blends were prepared by melt-mixing in a 50 ml Haake internal mixer with twin cam rotors, with the temperature of the mixing chamber initially set at 200°C and rotor speed set at 50 rpm. After mixing for 7 minutes under a constant flow of dry nitrogen, samples were immediately quenched in a bath of liquid nitrogen to freeze-in the morphology. A-1.2.4. Continuity measurement: Solvent extraction has been used to determine the composition region of co-continuity of the blends. As a primary advantage, solvent extraction is an absolute measurement (Steinmann, et al., 2001) and is capable of detecting the existence of co-continuous microstructures when the components are soluble in specific solvents (Potschke & Paul, 2003). The level of continuity of a phase in a sample is given by Equation A-1.2: Equation A-1.2 In this equation, minitial is the initial mass of the sample, mfinal is the final mass of the sample and minitial(i) is the mass of polymer i contained in the sample before selective extraction, calculated by considering the blend as homogeneous. Selective solvent extraction of the PMMA and PS phases were performed respectively in acetic acid and cyclohexane in a soxhlet extraction apparatus. Mass loss measurements were carried out for one week and were used to calculate the extent of continuity of the PMMA and PS phases using Equation A-1.2. A-1.2.5. Focused Ion Beam (FIB) preparation and Atomic Force Microscopy (AFM) morphology analysis: The specimens were initially cryomicrotomed to create a plane face using 239
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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
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
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: (Reignier & Favis, 2000, 2003a; Rei
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 and 302: Resistance(ohm) 1.0E+12 1.0E+11 1.0
Page 303 and 304: esistance value. Samples containing
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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