Crystallization Behavior of PS-PLLA Block Copolymers from Strong to Weak Segregation

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研究生：	許斐華
論文名稱：	Crystallization Behavior of PS-PLLA Block Copolymers from Strong to Weak Segregation
指導教授：	何榮銘
口試委員:
學位類別：	碩士 Master
系所名稱：	工學院 - 化學工程學系 Department of Chemical Engineering
論文出版年：	2007
畢業學年度：	96
語文別：	中文
論文頁數：	104
中文關鍵詞：	結晶性團聯高分子、聚苯乙烯與聚左旋乳酸、空間侷限尺寸
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In our previous work, crystallization from hard confinement to soft confinement under strong segregation strength in crystallizable block copolymer, poly(styrene)-block-poly(L-lactide) (PS-PLLA) (having Tg,PS ~ 85 °C, Tg,PLLA ~ 45 °C, Tm,PLLA ~ 150 °C), in microphase-separated lamellar morphology has been studied. An undulated morphology induced by crystallization in lamellar structure was observed in the PS13-PLLA24 block copolymer at Tc,PLLA > Tg,PS (i.e. soft confinement). In this study, a series of semicrystalline block copolymers PS-PLLA with lamellar microstructure were synthesized. A variety of PS-PLLA with different molecular weights, namely distinct segregated strength, were obtatined and crystallized from hard confinement (i.e., the crystallization temperature of PLLA (Tc,PLLA) < the glass transition temperature of PS (Tg,PS)) to soft confinement (i.e., Tc,PLLA>Tg,PS), where interesting morphological evolution was studied by transmission electron microscopy (TEM) and time-resolved small angle X-ray scattering (SAXS). A confined morphology for crystallized PS14-PLLA15 (high-molecular-weight samples) was observed at Tc,PLLA < Tg,PS , while at Tc,PLLA > Tg,PS, an undulated morphology was found. The effect of crystallization on microphase-separated lamellae suggests a strong dependence on the confined environments (i.e., Tg effect) justified by the ratio of Tc,PLLA and Tg,PS that plays a critical role in determining the ultimate morphology after the crystallization of PLLA. Compared to Tg effect, the effect of segregation strength on the morphological evolution is insignificant.
To further examine the effect of segregation strength on morphological evolution, a low-molecular-weight PS04-PLLA05 was synthesized. With the reduction of segregation strength in the PS-PLLA, undulated morphology was observed in both hard and soft confinement. To further examine the undulated morphology, the order-disorder transition temperature (TODT) of PS04-PLLA05 (i.e. low-MW samples) was determined by real-time SAXS heating experiments. The undulation of lamellae in the PS04-PLLA05 samples is initiated by the annealing at which the temperature is close to TODT; suggesting that the extent of thermal fluctuations causes the formation of lamellar undulation instead of crystallization event.
Furthermore, we explored polymeric crystallization mechanism under various nanoscale confined sizes by varying the molecular weight of PS-PLLA copolymer, namely the confined size. Compared to PLLA homopolymer, a significant variation of maximum crystallization-rate-
temperature (Tf) of PLLA block crystallized in PS-PLLA block copolymer can be identified because of the one-dimensional confinement effect. Furthermore, the dependence of crystallization halftime (t1/2) on Tc and dPLLA (i.e., confined size) was examined. Similarly, the increase in t1/2 was attributed to retardation of crystallization in PLLA blocks under 1-D confinement. Consequently, a significant decrease in crystallization rate is referred to the variation of confined size. In this study, however, a distinct transformation of isothermal crystallization kinetics, from heterogeneous to homogeneous nucleation, and a transformation in crystallographic orientation, from perpendicular to parallel type were not found even with the reduction of confined size. These results suggest that the confined size in all PS-PLLA block copolymers is not small enough to change the crystallization mechanism.

Abstract    I
Contents    IV
List of Tables     VI
List of Figures    VII
Chapter 1 Introduction    1
1.1 Self-Assembly    1
1.2 Self-assembly Behavior of Block Copolymers    2
1.3 Crystallization Effect on Semicrystalline Diblock Copolymers    5
1.3.1 Glass Transition Temperature Effect     6
1.3.2 Segregation Strength Effect    7
1.4 Fluctuation Effect on the Morphology of Block Copolymer    10
1.5 Confined Geometry Effect on Crystallization    11
1.6 Spatial Confinement Effect on Crystallization kinetics    12
1.7 Crystalline Orientation under Confinement    15
Chapter 2 Objectives    39
Chapter 3 Experimental    42
3.1 Instruments    42
3.2 Materials    42
3.2.1 Synthesis of PS-PLLA Block Copolymers    42
3.2.2 Preparation of PS-PLLA Diblock copolymers    42
3.3 The Orientation of Lamellar Structure    43
3.3.1 PS14-PLLA15 diblock copolymers (High-MW samples)    43
3.3.2 PS04-PLLA05 diblock copolymers (Low-MW samples)    43
3.4 Transmission Electron Microscopy (TEM)    44
3.5 Synchrotron X-ray Experiments    44
3.6 Differential Scanning Calorimetry (DSC)    46
Chapter 4 Results and Discussion     51
4.1 Lamellar Morphology of PS-PLLA with Various Molecular Weights………………………………………………………...51
4.2 Distinct Segregated Microphase Separation    52
4.3 Thermal Behavior of PS-PLLA Block Copolymers    53
4.4 Crystallization Effects under Distinct Segregated Strength    54
4.4.1 The Morphology of PS14-PLLA15 (High-MW Samples)    54
4.4.2 The Morphology of PS04-PLL05 (Low-MW Samples)    56
4.5 Fluctuation Effects on Morphology of PS-PLLA Block
   Copolymer    57
4.6 Crystal Orientation under Confinement    58
4.6.1 Crystal Orientation of PS14-PLLA15    58
4.6.2 Crystal Orientation of PS04-PLLA05    61
4.7 Crystallization under Various Nanoscale Confined Sizes    62
Chapter 5 Conclusions    96
Chapter 7 References    98


List of Tables
Table 3.1 Molecular characteristics of diblock copolymers and homopolymers.    48
Table 4.1 Long periods of PS-PLLA with different molecular weights    66
Table 4.2 Segregation strength ratios of PS-PLLA with different molecular weights.    67


List of Figures
Figure 1.1 Examples of static self-assembly. (a) Crystal structure of a ribosome. (b) Self-assembled peptideamphiphile nanofibers. (c) An array of millimeter sized polymeric plates assembled at a water/perfluorodecalin interface by capillary interactions. (d) Thin film of a nematic liquid crystal on an isotropic substrate. (e) Micrometersized metallic polyhedra folded from planar substrates. (f) A three-dimensional aggregate of micrometer plates assembled by capillary forces.    18
Figure 1.2 Examples of dynamic self-assembly. (a) An optical micrograph of a cell with fluorescently labeled cytoskeleton and nucleus; microtubules ~ 24 nm in diameter) are colored red. (b) Reaction-diffusion waves in a Belousov-Zabatinski reaction in a 3.5-inch Petri dish. (c) A simple aggregate of three millimeter-sized, rotating, magnetized disks interacting with one another via vortex-vortex interactions. (d) A school of fish. (e) Concentric rings formed by charged metallic beads 1 mm in diameter rolling in circular paths on a dielectric support. (f) Convection cells formed above a micropatterned metallic support. The distance between the centers of the cells is ~ 2 mm.    19
Figure 1.3 (a) Schematic phase diagram showing the various ‘classical’ BCP morphologies adopted by non-crystalline linear diblock copolymer. The blue component represents the minority phase and the matrix, majority phase surrounds it. (b) Schematic of morphologies for linear ABC triblock copolymer. A combination of block sequence (ABC, ACB, BAC), composition and block molecular weights provides an enormous parameter space for the creation of new morphologies. Microdomains are colored as shown by the copolymer strand at the top, with monomer types A, B and C confined to regions colored blue, red and green, respectively.    20
Figure 1.4 TEM micrographs showing the crystalline morphology of SEBS.    21
Figure 1.5 TEM micrographs of the PEO-b-PS sample after isothermally crystallized at 25oC    22
Figure 1.6 TEM micrographs showing the crystalline morphology of PEO-b-PB.    23
Figure 1.7 TEM micrographs showing the crystalline morphology of PE-b-PEE    24
Figure 1.8 Classification map of crystallization modes in semicrystalline diblocks with rubbery matrices. Open symbols represent samples where the melt mesophase was completely destroyed on cooling (breakout) or where the melt was homogeneous (unconfined); symbols with vertical hatch represent templated crystallization; and filled symbols represent confined crystallization. Circles represent diblocks forming spheres of E; squares represent cylinders. The bold dashed lines are guides to the eye, approximately dividing the region of breakout (bottom) from the region of confinement (top, light hatch) and the region of template crystallization (right center, heavy hatch).    25
Figure 1.9 TEM images of fully crystallized E/SEB after isothermal crystallization at 64 °C for 20 min. (a) (□Nt)c/(□Nt)ODT > 3 : confined morphology; (b) (□Nt)c/(□Nt)ODT < 3 : breakout morphology. SEB matrix is stained dark with RuO4    26
Figure 1.10 TEM images of fully crystallized PE-PMB system, oriented by channel die compression and crystallized on cooling at 10 °C/min: (a) confined cylinder; (b)templated cylinder; (c)breakout. Amorphous E and MB are both stained dark with RuO4. White ovals highlight “rogue” crystals which run between microdomains.    27
Figure 1.11 TEM micrographs of PS-sPP isothermally crystallized at (a) Tc,sPP < Tg,PS; (b) Tc,sPP ~ Tg,PS; and (c) Tc,sPP > Tg,PS    28
Figure 1.12 (a)Competition between the driving fore of crystallization and segregation strength of microphase separation. TEM micrographs of unoriented PS-PLLA samples (b) crystallized at 70 oC (c) crystallized at 100 oC from ordered melt at 160 oC    29
Figure 1.13 Schematic showing the variation of inverse scattering intensity and domain spacing across the order-disorder transition of a block copolymer melt. The mean field transition temperature has been identified operationally as the point where, on heating, the inverse intensity crosses over to a linear dependence on T-1    30
Figure 1.14 Illustration of lamellar deformation by rippling, and the associated changes in scattering patterns, as T □ TODT    31
Figure 1.15 Time course of the integrated SAXS (middle curve) and WAXS (bottom curve) intensities for E/SEB 63 crystallized at 67 oC (insets show regions of integration). The SAXS intensity for the E40 homopolymer, which shows a sigmoidal time evolution, is shown for comparison (top curve, 95 oC, similar half-time)    32
Figure 1.16 Nonisothermal crystallization exotherms of PEO-b-PBs. The cooling rate was 5 °C/min. The inset in the figure plots the freezing temperature (Tf) as a function of fPB. It can be seen that the crystallization kinetics exhibits transitions at the compositions corresponding to the morphological transformation    33
Figure 1.17 ((a) Dependence of half-time of isothermal crystallization on temperature and (b) lamellar thickness, lCPCL, of crystalline PCL stems as a function of Tc for P4VP-PCL BCPs and PCL homopolymers. Horizontal lines denote the confined sizes. The characteristic thicknesses of crystalline PCL stems for BCPs were estimated from plots of inverse crystal lamellar thickness vs melting temperature from evolution of SAXS data.    34
Figure 1.18 TEM micrographs showing the crystalline morphology of SEBS.    35
Figure 1.19 (a) Parallel; (b) Perpendicular orientation in confined cylinder    36
Figure 1.20 (a) Homogeneous/ parallel orientation; (b) homeotropic/ perpendicular orientation in confined lamellar nanostructures    37
Figure 1.21 (a) Three schematic presentations of chains orientation under confinement with various spaces in the P4VP-b-PCL diblock copolymers: (a) dPCL~11nm, (b) dPCL~8.8nm, and (c) dPCL~6nm.    38
Figure 3.1 PS-PLLA double-headed polymerization sequences.    47
Figure 3.2 Illustration of rimming flow and the orientation of lamellar microstructure    49
Figure 3.3 Geometry of the mechanical sheared PS04-PLLA05 copolymers with a lamellar phase morphology    50
Figure 4.1 (a) TEM morphology; (b) The corresponding azimuthally integated one-dimensional SAXS profile of PS14-PLLA15 (fPLLAv = 0.49) after quenching from 160 °C    68
Figure 4.2 (a) TEM morphology; (b) The corresponding azimuthally integated one-dimensional SAXS profile of PS07-PLLA11 (fPLLAv = 0.58) after quenching from 160 °C.    69
Figure 4.3 (a) TEM morphology; (b) The corresponding azimuthally integated one-dimensional SAXS profile of PS04-PLLA05 (fPLLAv = 0.51) after quenching from 160 °C    70
Figure 4.4 (a) TEM morphology; (b) The corresponding azimuthally integated one-dimensional SAXS profile of PS06-PLLA05 (fPLLAv = 0.37) after quenching from 160 °C    71
Figure 4.5 One-dimensional SAXS profile of PS-PLLA copolymers with different molecular weights    72
Figure 4.6 DSC heating thermograms of (a) PS14-PLLA15 (fPLLAv = 0.49) and (b) PS04-PLLA05 (fPLLAv = 0.51). The heating rate is 10oC/min    73
Figure 4.7 DSC heating thermograms of (a) PS14-PLLA15 (fPLLAv = 0.49) and (b) PS04-PLLA05 (fPLLAv = 0.51). The heating rate is 10oC/min    74
Figure 4.8 DSC thermograms of (a) isothermal crystallization; (b) melting curves for PS14-PLLA15 (fPLLAv = 0.49) at different crystallization temperatures. On the basic reciprocal time of exothermic peak, the maximum crystallization rate is estimated at ca. 95 oC. The melting point increases with increasing crystallization temperature    75
Figure 4.9 DSC thermograms of (a) isothermal crystallization; (b) melting curves for PS04-PLLA05  (fPLLAv = 0.51) at different crystallization temperatures. On the basic reciprocal time of exothermic peak, the maximum crystallization rate is estimated at ca. 110 oC. The melting point increases with increasing crystallization temperature.    76
Figure 4.10 Crystallization of PS-PLLA from hard to soft confinement under strong segregation strength    77
Figure 4.11 (a) TEM morphology; (b) one-dimensional SAXS profile of PS14-PLLA15 (fPLLAv = 0.49) isothermally crystallized at 70oC for 150 min from ordered melt at 160 oC. (Tc,PLLA = 70oC < Tg,PS = 87oC, under hard confinement)    78
Figure 4.12 (a) TEM morphology; (b) one-dimensional SAXS profile of of PS14-PLLA15 (fPLLAv = 0.49) isothermally crystallized at 100oC for 150 min from ordered melt at 160 oC. (Tc,PLLA = 100oC > Tg,PS = 87oC, under soft confinement)    79
Figure 4.13 (a) TEM morphology; (b) one-dimensional SAXS profile of of PS04-PLLA05 (fPLLAv = 0.51) isothermally crystallized at 70oC for 600 min from ordered melt at 160 oC. (Tc,PLLA = 70oC < Tg,PS = 87oC, under hard confinement)    80
Figure 4.14 (a) TEM morphology; (b) one-dimensional SAXS profile of PS04-PLLA05 (fPLLAv = 0.51) isothermally crystallized at 100oC for 200 min from ordered melt at 160 oC. (Tc,PLLA = 100oC > Tg,PS = 84oC, under soft confinement).    81
Figure 4.15 Real-time temperature dependence of SAXS profiles for PS04-PLLA05 in the heating process at various temperatures.    82
Figure 4.16 The plots of Im-1 versus 1/T for PS04-PLLA05    83
Figure 4.17 X-ray scattering patterns of oriented PS14-PLLA15 samples isothermally crystallized at 70 oC from ordered melt. 2-D SAXS obtained when X-ray beam is along (a) X-direction; (b) Y-direction; (c) Z-direction; 2-D WAXD along (d) X-direction; (e) Y-direction; (f) Z-direction.    84
Figure 4.18 (a) Azimuthal profiles for 2-D WAXD pattern of oriented PS14-PLLA15 samples isothermally crystallized at 70 oC from ordered melt along X-direction and Y-direction, respectively. (b) Schematic illustration of corresponding reflections    85
Figure 4.19 X-ray scattering patterns of oriented PS14-PLLA15 samples isothermally crystallized at 100 oC from ordered melt. 2-D SAXS obtained when X-ray beam is along (a) X-direction; (b) Y-direction; (c) Z-direction; 2-D WAXD along (d) X-direction; (e) Y-direction; (f) Z-direction    86
Figure 4.20 Azimuthal profiles for 2-D WAXD pattern of oriented PS14-PLLA15 samples isothermally crystallized at 100 oC from ordered melt along X-direction and Y-direction, respectively    87
Figure 4.21 Molecular disposition of PLLA crystalline chain corresponding to the lamellar interface for PS14-PLLA15 block copolymer    88
Figure 4.22 X-ray scattering patterns of oriented PS04-PLLA05 samples isothermally crystallized at 70 oC from ordered melt. 2-D SAXS obtained when X-ray beam is along (a) X-direction; (b) Y-direction; (c) Z-direction; 2-D WAXD along (d) X-direction; (e) Y-direction; (f) Z-direction    89
Figure 4.23 X-ray scattering patterns of oriented PS14-PLLA15 samples isothermally crystallized at 100 oC from ordered melt. 2-D SAXS obtained when X-ray beam is along (a) X-direction; (b) Y-direction; (c) Z-direction; 2-D WAXD along (d) X-direction; (e) Y-direction; (f) Z-direction    90
Figure 4.24 X-ray scattering patterns of oriented PS04-PLLA05 samples isothermally crystallized at 100 oC from ordered melt. 2-D SAXS obtained when X-ray beam is along (a) X-direction; (b) Y-direction; (c) Z-direction; 2-D WAXD along (d) X-direction; (e) Y-direction; (f) Z-direction    91
Figure 4.25 Azimuthal profiles for 2-D WAXD pattern of oriented PS04-PLLA05 samples isothermally crystallized at 100 oC from ordered melt along X-direction and Y-direction, respectively    92
Figure 4.26 Non-isothermal crystallization of (a) PLLA homopolymers and (b) PS-PLLA block copolymers with different molecular weight    93
Figure 4.27 Isothermal crystallization of PS-PLLA block copolymers with different confined sizes    94
Figure 4.28 Development of crystallinity during isothermal crystallization at different Tc from hard confinement and soft confinement in all PS-PLLA block copolymers. (a) Tc is at 70 oC  (b) Tc is at 100 oC. The relative crystallinity was deduced from the enthalpy change during dynamic isothermal crystallization in a DSC    95

                                

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