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研究生： 孫亞賢
Sun, Ya-Sen
論文名稱： 半結晶性高分子系之多晶態，熔融行為及熱誘導相轉變機制之探討：間規排向聚苯乙烯
Polymorphism, Thermal Behavior and Phase Transitions as a Function of Temperature in Semicrystalline Syndiotactic Polystyrene
指導教授： 吳逸謨
Woo, E. M.
學位類別： 博士
Doctor
系所名稱： 工學院 - 化學工程學系
Department of Chemical Engineering
論文出版年： 2002
畢業學年度： 90
語文別： 英文
論文頁數： 161
中文關鍵詞： 多晶態 、相轉變 、間規排向聚苯乙烯 、熱行為
外文關鍵詞： polymorphism, thermal behavior, phase transition, syndiotactic polystyrene
相關次數： 點閱：120  下載：8 
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    • 中文摘要
    本研究利用傅立葉紅外光光譜儀、廣角X光繞射分析儀、微分掃描熱卡計、穿透式電子顯微鏡、電子繞射、掃描式電子顯微鏡及偏光顯微鏡研究間規排向聚苯乙烯之溶劑誘導結晶及熱誘導結晶之多晶態、熱行為及相轉變機制之探討。研究發現不同溶劑誘導結晶或是溶於溶劑成膜形成不同的d晶態。本研究所使用的溶劑有三種，分別為四氯乙烷、二氯乙烷、及鄰位二氯苯。利用將試樣溶於四氯乙烷後成膜發現不需升溫過程直接形成g晶態，當溫度高於200°C時，發生g晶態轉變為a¢晶態。然而含有溶劑之試樣在高溫中直接轉變為b晶態。而對於二氯乙烷及鄰位二氯苯，則溶劑誘導結晶形成d晶態，利用升溫將溶劑揮發，則發現分別形成disordered及ordered的g晶態。Ordered的g晶態在200°C高溫轉變為a¢晶態，而disordered的g晶態在160°C轉變為a¢晶態。除此之外，對於冷結晶研究結果，由不定形慢速升溫發現，mesomorphic form先形成，在200°C高溫經由固態-固態相轉變程序轉變為a¢晶態。再者，對於多晶態與多熔峰的探討。對於b-type晶態，已知在230°C結晶形成三個熔融峰，熔融溫度分別252.3(P-I)，265.0(P-II)及271.0°C(P-III)，利用掃描式電子顯微鏡(SEM)觀察可知P-I為flat-on晶板排列，而P-II為two-eyes結構晶板之熱行為，而對於P-III則為亞穩態flat-on的晶板經過升溫掃描後熔融再結晶形成較穩定且較厚的edge-on晶板。低溫形成flat-on的晶板及two-eyes結構的晶板，而在高溫中則形成edge-on晶板結構。對於冷結晶形成的a晶態，可知在150°C結晶形成a¢-type晶態，為較小的球晶(finny spherulites)，而對於260°C結晶形成a²-type晶態，為sheaf-like的球晶形態。而對於熱行為可知，在150°C結晶形成a¢-type晶態，其熔融峰為單一且寬廣的熔融峰，而對於260°C結晶形成a²-type晶態，則形成雙熔融峰熱行為。

    Abstract
    The first portion of this dissertation focuses on solution-cast and solvent-induced crystallization. To investigate the phase transitions of the sPS-solvent complexes of d or g-crystals subjected to slow heating, three solvents are used in this study: 1,1,2,2-tetrachloroethane, o-dichlorobenzene and 1,2-dichloroethane. According to evidences of X-ray diffraction, transmission electron microscopy, electron diffraction, differential scanning calorimeter combined with Fourier transform infrared analysis, we have confirmed that the g-type crystal is directly yielded without further annealing by solution-cast for sPS/1,1,2,2-tetrachloroethane system, while the similar sample preparations imposed on sPS samples produce d-type crystal for sPS/o-dichlorobenzene and sPS/1,2-dichloroethane systems. Through TEM morphological observation, one has found the small crystallizes of g-form with typical size of <100nm. The TEM morphology and powder-like ED patterns of g-from are shown in Chapter 2. Additionally, upon annealing, two possible helix®trans phase transitions are successfully proposed by using the IR spectral changes in the frequency range of 720~820cm-1 which is associated with the vibration of the C-H out of plane bending of the phenyl ring. On is that an ordered g-type®a¢-type crystal transition occurs at a high temperature of about 200°C. The other is that a disordered g-type®a¢-type crystal transition occurs at approximate 160°C. The detail results are discussed in Chapter 3. Furthermore, on the basis of the IR spectra changes as a function of rising annealing temperature, the degree of crystallinity of mesomorphic form was quantitatively evaluated and determined. A temperature-induced solid-solid transition from mesomorphic form to a¢-crystal has been confirmed. An effect of the miscible blends with various contents of aPS on the polymorphism of the sPS sample subjected to cold-crystallization is also discussed in the study. It has been found that mixed a and b-crystals of various fractions was obtained in the sPS/aPS blends while the a-crystal (or mesomorphic form) becomes discernible species in the glassy sPS samples subjected to cold-crystallization. However, there is no miscible blends effect on a g-type®a¢-type crystal transition by slow heating the solution-cast sPS/aPS blends. Several reasonable models for explanations on structural changes with rising annealing temperatures were also proposed in the text.
    The second portion of this study focuses on the morphological changes in the sPS samples melt and cold-crystallized isothermally at various temperatures. It has been known that the sPS samples possess multiple melting behaviors. According to the evidences of polarized microscopy, scanning electron microscopy, X-ray diffraction and differential scanning calorimeter, a correlation between lamellar morphology and multiple melting peaks are clarified. There are three melting peaks, which are assigned as P-I, P-II and P-III, in the sPS samples consisting of isolated b¢-type crystal when melt-crystallized at a low temperature of 230°C. A morphology analysis showed that flat-on lamellae develop first, which yield P-I and P-II melting, and during scanning re-crystallize to thickened edge-on lamellae with P-III melting peak. Upon scanning, melting of P-I (crystal of the lowest melting peak) is followed by repacking into thickened P-III crystal, the lamellae of which also reoriented to a perpendicular orientation. The P-II crystal, however, melts at temperatures too close to the melting temperature of P-III; thus, during scanning up, the P-II crystal simply melts without sufficient time to repack into the thickened P-III crystal. In addition, P-III lamellae could also be directly developed in sPS by melt-crystallization at higher temperatures while P-I and P-II crystals were absent. Cold-crystallization of sPS produced only a-type unit cell peaked into crystalline domains of different morphology. The morphology contains a granular-sphere texture when cold-crystallized at low temperatures while high-temperature cold-crystallization produced additional sheaf-like lamellae radiating out from the central spheres.

    ABSTRACT (English and Chinese) I ACKNOWLEDGEMENT IV CONTENT V LIST OF FIGURES IX PART I CHAPTER 1 INTRODUCTION 1 1.1 Polymorphism 1 1.1.1 mesomorphic form, a- and b-crystals in thermal-crystallized sPS samples 1 1.1.2 d-crystals in solvent-crystallized sPS samples 4 1.2 Multiple melting behavior 6 1.3 Phase transitions 8 1.4 References 10 CHAPTER 2 CRYSTAL TRANSFORMATION AND STRUCTURAL CHANGES IN SOLVENT-CAST THIN-FILM SYNDIOTACTIC POLYSTYRENE CONTAINING 1,1,2,2-TETRACHLOROETHANE (Cl2CHCHCl2) 13 2.1 Introduction 14 2.2 Experimental 17 2.2.1 Materials and Procedures 17 2.2.2 Apparatus 18 2.3 Results and Discussion 19 2.3.1 X-ray diffraction pattern of unoriented sample 19 2.3.2 Electron diffraction and morphology of the g-type crystal 21 2.3.3 Thermal behavior by DSC 21 2.3.4 WAXD characterization of phase transition 22 2.3.5 IR characterization of phase transition 23 2.3.6 Molecular structural changes depending on rising annealing temperature 26 2.3.7 Solvent effect on the chains packed in the zigzag conformation 28 2.4 Summary 30 2.5 References 30 CHAPTER 3 INFRARED SPECTROSCOPY STUDY ON CRYSTAL AND TEMPERATURE DEPENDENCE STRUTURAL CHANGES IN SYNDIOTACTIC POLYSTYRENE CONTAINING 1,2-DICHLOROETHANE and O-DICHOROBENZENE UPON THERMAL-INDUCTION 48 3.1 Introduction 49 3.2 Experimental 50 3.2.1 Materials and Procedures 51 3.2.2 Apparatus 51 3.3 Results and Discussion 52 3.3.1 X-ray diffraction pattern of unoriented samples 52 3.3.2 Calorimetric investigations of d-type crystals 52 3.3.3 WAXD characterization of phase transition 53 3.3.4 IR characterization of phase transition 54 3.3.5 Molecular structural changes depending on rising annealing temperature 57 3.3.6 Phase transition mechanisms 61 3.4 Summary 61 3.5 References 62 CHAPTER 4 QUANTITATIVE EVALUATION OF CRYSTALLINITY AND PHASE TRANSITION OF PLANAR MESOMORPHIC FORM IN SYNDIOTACTIC POLYETYRENE BY USING FTIR SPECTRUM 78 4.1 Introduction 79 4.2 Experimental 81 4.2.1 Materials and Procedures 81 4.2.2 Apparatus 82 4.3 Results and Discussion 83 4.3.1 Quantitative determination of crystallinity of the mesomorphic form 83 4.3.2 IR characterization of phase transition when slow heating upon quenched glassy samples 86 4.3.3 WAXD characterization of phase transition 89 4.3.4 IR characterization of phase transition when slow heating upon the quenched glassy samples and its blends 91 4.3.5 IR characterization of phase transition when slow heating upon the solution-cast blends 94 4.4 Summary 95 4.5 Reference 96 Part II CHAPTER 5 CORRELATION BETWEEN THERMAL BEHAVIOR AND CRYSTALLINE MORPHOLOGY IN b-FORM SYNDIOTACTIC POLYSTYRENE 122 5.1 Introduction 122 5.2 Experimental 123 5.2.1 Materials and Procedures 123 5.2.2 Apparatus 123 5.3 Results and Discussion 123 5.3.1 Unit cell crystals 123 5.3.2 Lamellar/Spherulite morphology 125 5.3.3 Multiple melting of lamellae 126 5.3.4 Mechanism of lamellar re-organization 128 5.3.5 Discussion on correlation between melting and morphology 129 5.4 Summary 132 5.5 References 132 CHAPTER 6 MECHANISM OF REORGANIZATION OF LAMELLAE IN SYNDIOTACTIC POLYSTYRENE 134 6.1 Introduction 134 6.2 Experimental 135 6.3 Results and Discussion 136 6.4 Summary 144 6.5 References 145 CHAPTER 7 MORPHOLOGY AND CRYSTAL STRUCTURE OF COLD-CRYSTALLIZED SYNDIOTACTIC POLYSTYRENE 146 CHAPTER 8 TEMPERATURE AND CCOMPOSITION EFFECTS ON POLYMORPHISM CHANGES IN COLD-CRYSTALLIZED MISCIBLE BLENDS OF SYNDIOTACTIC AND ATACTIC POLYSTYRENES 151 CHAPTER 9 CONCLUSION 156 PAPER PUBLICATIONS & VITA 158

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    Charpter 2
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