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Phase continuity (%) 100 90 80 70 60 50 40 30 20 10 0 Continuity of PMMA Continuity of PMMA+PS Continuity of PS (a) (b) (c) (d) (e) (f) 0 20 40 60 80 100 Volume fraction of HDPE(HDPE+PVDF = 70% of total) Figure 4-9. Continuity level of PS, PMMA, and PS+PMMA obtained by solvent extraction/gravimetry for 6 blends comprised of HDPE/PS/PMMA/PVDF; (a) 10/15/15/60, (b) 20/15/15/50, (c) 30/15/15/40, (d) 40/15/15/30, (e) 50/15/15/20, (f) 60/15/15/10. Selective extraction associated with gravimetric measurements was carried out to obtain the continuity levels of PS, PMMA, and PS+PMMA in order to determine the concentrations where the phases are continuous. The continuity of HDPE and PVDF were estimated based on SEM photomicrographs at various compositions. Gravimetric results exhibit a low level of continuity (ranging from five to fifteen percent) for all phases in a 10/15/15/60 HDPE/PS/PMMA/PVDF onion morphology. Increasing the concentration of HDPE to 20 parts in the blend with PVDF at 50 (28.6% HDPE on the x-axis) yields a hierarchical-layered morphology with an HDPE core where the continuity of PS and PMMA reaches levels of 30% and 43%, respectively. Further increasing the HDPE concentration results in a maximum continuity of all phases for blends of 30/15/15/40 HDPE/PS/PMMA/PVDF and 40/15/15/30 HDPE/PS/PMMA/PVDF (Figure 4-9). If 120
the concentration of HDPE is increased further, an inverse behavior is observed where PVDF becomes the core and HDPE becomes the matrix. In this case, for the blend containing 50HDPE/15PS/15PMMA/20PVDF, the continuity of middle phases including PS and PMMA becomes 15% and 30%, respectively. Figure 4-9 shows that when the concentration of HDPE is increased up to 60 parts in the blend, the continuity of PS and PMMA becomes less than five percent. 4.4.4 Generating Highly Continuous Quinary Polymer Blends In this part of the work, the addition of a fifth component to the highly continuous quaternary blends ranging from 30/15/15/30 to 40/15/15/30 HDPE/PS/PMMA/PVDF, selected from the previous section, is examined. Ten percent PANI is added to a quaternary blend of HDPE/PS/PMMA/PVDF within the region of multi-percolation resulting in the formation of a five-component blend of 30/15/15/30/10 HDPE/PS/PMMA/PVDF/PANI(Figure 4-10). Figure 4-10a shows the continuous HDPE phase after the removal of all other phases. The selective extraction of PMMA and PS reveals a perfectly homogeneous continuous network for those phases in the blend (Figure 4-10b and Figure 4-10c). The extraction of both PS and PMMA phases together separates the multi-blend into two inter-diffused continuous structures where one of them is a continuous HDPE phase and the other is a continuous PANI and PVDF phase (Figure 4-10d). It also illustrates that continuous networks of PS and PMMA are adjacent to each other. In Figure 4-10e, the network of PANI which has been extracted by chromic acid is clearly detected. In order to unambiguously illustrate that PANI forms a network morphology, blends of 25/25/25/25 PS/PMMA/PVDF/PANI and 15/20/15/25/25 PS/PS-co- PMMA/PMMA/PVDF/PANI are prepared. The influence of the addition of a PS-co-PMMA copolymer on the segregation of phases is discussed in a following section in detail. After the extraction of all phases except PANI and followed by a freeze-drying process, a network of PANI with very thin walls remains, as represented in Figure 4-11. Freeze-drying is carried out to prevent of shrinkage of the PANI network. 121
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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
Page 115 and 116: on the topic have been reported in
Page 117 and 118: succeeded in creating thin films wi
Page 119 and 120: Addition of salt to the solution of
Page 121 and 122: different from that of linear homop
Page 123 and 124: Figure 2-39. Macromolecule with a)
Page 125 and 126: polyanion such as hyaluronan (HA)(P
Page 127 and 128: 2.4.1.1.7 Effect of Salt on Multila
Page 129 and 130: 2.4.1.1.8 Overcompensation of the M
Page 131 and 132: important factors determining the g
Page 133 and 134: As shown in Figure 2-44, swelling a
Page 135 and 136: increasing the pH value due to a de
Page 137 and 138: CHAPTER 3 - ORGANIZATION OF THE ART
Page 139 and 140: discussed above, HDPE, PS, PMMA, an
Page 141 and 142: CHAPTER 4 - LOW PERCOLATION THRESHO
Page 143 and 144: or model which predicts where the p
Page 145 and 146: concentration threshold for the ons
Page 147 and 148: 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: Uniform layers of PS and PMMA situa
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 and 214: In this work the conductance of the
Page 215 and 216: 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
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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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