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The final part of the work focuses on the complex morphological structures which can be generated from a ternary polymer blend demonstrating complete wetting behavior. This work examines the complete range of possible morphological states for such a system over the entire ternary composition diagram as prepared by melt mixing. A ternary polymer blend comprised of HDPE, PS, and PMMA is selected as a model system demonstrating complete wetting. The positive spreading coefficient of λPS/PMMA=2.6 mN/m indicates that PS separates the HDPE and PMMA phases. Four thermodynamically stable sub-categories of morphologies can be identified: a) matrix/core-shell dispersed phase; b) tri-continuous; c) bi-continuous/dispersed phase; and d) matrix/two separate dispersed phases. Electron microscopy as well as focused ion beam irradiation and atomic force microscopy are used to clearly illustrate and identify the various phases. Solvent extraction/gravimetry is used to examine the extent of continuity of the systems so as to effectively identify regions of high continuity. Triangular compositional diagrams are used to distinguish these various morphological regions and the results are interpreted in light of the interfacial tension of the various binary combinations and their subsequent spreading coefficients. The effect of the molecular weight and viscosity ratio on the phase size of the various structures is also considered. It is shown that the viscosity of the phases can influence the interfacial area between phases, but does not affect the morphological state classification. xii
CONDENSÉ EN FRANÇAIS Dans ce travail, nous avons étudié la morphologie de mélanges à plusieurs composants préparés à l’état fondu, suivi de gravure par solvant, afin de générer de nouveaux dispositifs conducteurs avec un seuil de percolation extrêmement faible. Cette thèse mesure et élabore sur l’évolution de la continuité dans les morphologies co-continues à percolation double, triple et quadruple, dans le but de trouver le moyen de réduire considérablement le seuil de percolation de toutes les phases dans le mélange. L’utilisation de structures continues dans les mélanges polymères constitue une manière élégante de réduire la continuité et/ou le seuil de percolation électrique d’un polymère conducteur. À cette fin, le polyaniline (PANI) et quatre autres polymères, disponibles commercialement, avec les tensions de surface, les polarités et les tensions interfaciales désirées, sont sélectionnés. Les tensions interfaciales entre les différents composants se situent dans une plage variant entre 1 mN/m, pour le PVDF/PMMA, et 26,9 mN/m, pour le PANI/HDPE. La caractérisation morphologique des échantillons est effectuée en utilisant la microscopie électronique à balayage (MEB) et le faisceau ionique focalisé (FIF) couplé à la microscopie par force atomique (MFA). Les mélanges polymères sont préparés à l’état fondu dans un mélangeur interne, à 50 tr/min pendant 8 minutes à 200°C. L’extraction sélective des phases par solvant est utilisée, soit pour aider à mieux distinguer les phases afin de recueillir de l’information qualitative, soit pour produire des échantillons poreux. La combinaison du traitement par FIF et de la MFA permet de distinguer clairement les phases à partir du contraste topographique résultant de la différence des taux de gravure des matériaux par FIF. Afin d’étudier l’effet du ratio de viscosité dans les mélanges ternaires, deux polyméthacrylates de méthyle (PMMA) sont choisis pour leurs masses moléculaires différentes. Des matériaux poreux entièrement interconnectés sont utilisés comme substrats pour la déposition alternée de PSS et de PANI. Dans la première étape, trois composants, soit le polyéthylène à haute densité (HDPE), le polystyrène (PS) et le PMMA sont soigneusement sélectionnés pour satisfaire les conditions thermodynamiques. Le coefficient d’étalement positif λPS/PMMA = 2,6 mN/m, basé sur les trois tensions interfaciales des paires de polymères (HDPE/PS (γPS/HDPE = 4,7 mN/m), PS/PMMA (γPS/PMMA = 1,1 mN/m), et HDPE/PMMA (γHDPE/PMMA = 8,4 mN/m)), prévoit que la phase de PS xiii
Page 1 and 2: © Sepehr Ravati, 2010. UNIVERSITÉ
Page 3 and 4: DEDICATED To my parents iii
Page 5 and 6: RÉSUMÉ Cette thèse présente, po
Page 7 and 8: devenir une structure hiérarchique
Page 9 and 10: ABSTRACT This thesis presents, for
Page 11: system can be increased from 10 -15
Page 15 and 16: deuxième coquille de PS. Les phase
Page 17 and 18: structures à percolation multiple
Page 19 and 20: autre sous-type de morphologie dans
Page 21 and 22: TABLE OF CONTENTS DEDICATION.......
Page 23 and 24: xxiii 2.4.1.1.1 Charged Polymer Ads
Page 25 and 26: 5.3.4 Annealing Test ..............
Page 27 and 28: xxvii REFERENCES ..................
Page 29 and 30: LIST OF FIGURES xxix Figure 1-1. a)
Page 31 and 32: Figure 2-12. SEM photomicrograph of
Page 33 and 34: Figure 2-34. Schematic view of diff
Page 35 and 36: Figure 4-8. SEM micrographs of vari
Page 37 and 38: Figure 5-6. a),b) Scanning electron
Page 39 and 40: and c) triangular concentration dia
Page 41 and 42: n number of moles p concentration o
Page 43 and 44: AFM atomic force microscopy LIST OF
Page 45 and 46: PS-co-PMMA copolymer of PS and PMMA
Page 47 and 48: 1.1 Introduction CHAPTER 1 - INTROD
Page 49 and 50: Figure 1-2. Human heart, longitudin
Page 51 and 52: One of the applications for porous
Page 53 and 54: On the other hand, a novel tri-cont
Page 55 and 56: 2.1 Polymer Blends CHAPTER 2 - LITE
Page 57 and 58: Based on Sterling’s approximation
Page 59 and 60: Antonoff’s rule (Equation 2-13) i
Page 61 and 62: 2.1.2.1 Binary Polymer Blends 2.1.2
Page 63 and 64:
Some other studies(Everaert, Aerts,
Page 65 and 66:
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
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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
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,
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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
Page 289 and 290:
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
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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