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研究生：	張桔源 Chang, Chieh-Yuan
論文名稱：	藉由結構工程結合交聯與環烷設計優化聚醯亞胺之介電與電化學特性 Optimizing Dielectric and Electrochemical Properties of Polyimides by Structural Engineering Using Crosslinking and Alicyclic Designs
指導教授：	林彥丞 Lin, Yan-Cheng
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：	2025
畢業學年度：	113
語文別：	英文
論文頁數：	168
中文關鍵詞：	聚醯亞胺、交聯、高頻介電材料、區段共聚、陽離子交換薄膜、釩液流電池
外文關鍵詞：	polyimide polymers, crosslinking, high-frequency dielectric materials, block copolymerization, proton exchange membranes, vanadium redox flow batteries
相關次數：	點閱：17 下載：1
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本研究針對兩類高性能高分子材料—聚醚醯亞胺（PEI）與磺化聚醯亞胺（SPI）薄膜，進行結構設計、功能調控與系統性性能評估，目標為開發適用於高頻電子與儲能應用的關鍵材料。針對PEI薄膜，採用後交聯策略，於聚合後進行甲醇脫除反應以建立穩定的三維網絡結構，有效兼顧前驅體的溶解性與薄膜的成型性。實驗結果顯示，BAPHF主鏈薄膜在1 mol%交聯條件下，不僅具備優異的熱穩定性（Td5% = 519 °C, CTE = 68 ppm/K）、機械剛性與光學透明性，亦於29–38 GHz頻段展現出極低的介電常數（2.52），為兼具多重性能的理想薄膜設計。在SPI薄膜部分，透過引入具剛性與非共平面結構的脂環二胺TCDDA，並與磺化二胺進行區段共聚，有效提升微相分離與自由體積比例，進而大幅降低釩離子通透率（9.79×10⁻⁸ cm²/min）並提高庫倫效率（CE > 90%）。T10膜更於實際VRFB電池測試中展現優異的能量效率與長期循環穩定性，顯示其卓越的選擇性與耐久性。綜上所述，本研究透過分子設計與交聯／共聚策略，成功開發出具備熱穩定性佳、結構完整、並具介電與離子選擇性的高功能性高分子薄膜，對於次世代電子與能源應用具有高度潛力。

This study focuses on the structural design, functional tuning, and systematic performance evaluation of two types of high-performance polymer materials—polyetherimide (PEI) and sulfonated polyimide (SPI) thin films—with the goal of developing key materials for high-frequency electronics and energy storage applications. For PEI films, a post-crosslinking strategy was adopted, in which methanol elimination reactions were conducted after polymerization to form stable three-dimensional networks. This approach effectively balances the solubility of the precursor with subsequent film processability. Experimental results show that the BAPHF-based PEI film with 1 mol% crosslinking exhibits an ideal combination of thermal stability, mechanical rigidity, optical transparency, and the lowest dielectric constant in the 29–38 GHz range. In the case of SPI films, the introduction of the rigid and non-coplanar alicyclic diamine TCDDA via segmental copolymerization enhanced microphase separation and increased free volume, significantly reducing vanadium ion permeability (9.79×10⁻⁸ cm²/min) and improving coulombic efficiency (CE > 90%). The T10 membrane also demonstrated excellent energy efficiency and long-term cycling stability in practical VRFB testing, indicating outstanding selectivity and durability. In summary, this study successfully developed functional polymer films with balanced thermal stability, structural integrity, and dielectric/ion-selective properties through molecular design and crosslinking/copolymerization strategies, offering significant potential for next-generation electronic devices and energy systems.

中文摘要 i
ABSTRACT ii
誌謝 iii
CONTENT	iv
LIST OF FIGURES	viii
LIST OF TABLES xiii
LIST OF SCHEMES	xiv
LIST OF ABBREVIATION xv
Chapter 1. Introduction	1
1-1 Preface 1
1-2 Polyimides (PIs) 3
1-2-1 Molecular Structure and Classification 4
1-2-2 Synthetic Approaches of PIs 5
1-2-3 Applications of Polyimides 8
1-3 Dielectric Properties 10
1-3-1 Dielectric Proprties and Polarization Mechanism 10
1-3-2 The factors that influence Dk of polyimides 11
1-3-2-1 Frequency and temperature effect 11
1-3-2-2 Polarizability 14
1-3-2-3 Molecular structures 15
1-3-2-4 Polar Functional Groups and Dipole Density 16
1-3-2-5 Free Volume and Density 18
1-3-3 The factors that influence Df of polyimides 21
1-3-3-1 Dipole Moment 21
1-3-3-2 Chain Flexibility and Segmental Mobility 23
1-3-3-3 Water Uptake 24
1-4 Strategies for Improving Dielectric Properties of Polyimides 25
1-4-1 Strategies for Reducing Dk 25
1-4-1-1 Incorporation of Fluorinated Moieties 25
1-4-1-2 Introduction of Bulky and Noncoplanar Rigid Structures 27
1-4-1-3 Use of Alicyclic and Semi-Alicyclic Monomers 28
1-4-1-4 Crosslinking and Network Architecture 29
1-4-2 Strategies for Reducing Df 31
1-4-2-1 Rigid Structures 31
1-4-2-2 Hydrophobic Design 32
1-5 PI-based Proton Exchange Membrane (PI-based PEMs) 34
1.5.1 Fundamental Requirements of Proton Exchange Membranes 34
1.5.2 Sulfonated Polyimides 35
1.5.3 Structural Design Strategies for Enhancing Performance 37
1.5.4 Comparison with Other Emerging PEM Materials 39
1-6 PI-based PEMs in Vanadium Redox Flow Batteries (VRFBs) 41
1.6.1 Vanadium Redox Flow Batteries 41
1.6.2 Design Criteria for PEMs in VRFBs 44
1.6.3 Structural Design Strategies for PI-based PEMs for VRFBs 46
1.6.4 Performance Comparison with Nafion in VRFBs 48
1-7 Research Objectives 49
Chapter 2. Experimental Method 52
2-1 Experimental Chemicals 52
2-2 Experimental Details and Procedure 54
2-2-1 Synthesis and Film Preparation of Crosslinked Polyimides 54
2-2-1-1 Synthesis of the Linear Polyetherimide (PEI) 54
2-2-1-2 Synthesis of the Crosslinked PEIs 55
2-2-2 Synthesis and Membrane Preparation of Alicyclic-Structured Polyimides 56
2-2-2-1 Purification of BDSA 56
2-2-2-2 Synthesis of the Nonalicyclic Block Copolymer PEM 57
2-2-2-3 Synthesis of the Alicyclic-Containing Block Copolymer PEM 58
2-3 Experimental Equipment and Instruments 59
2-3-1 Nuclear Magnetic Resonance (NMR) 60
2-3-2 Fourier Transform Infrared Spectroscopy (FTIR) 61
2-3-3 Gel Permeation Chromatography (GPC) 62
2-3-4 Capillary Viscometer 64
2-3-5 Density Meter 65
2-3-6 Thermogravimetric Analysis (TGA) 66
2-3-7 Differential Scanning Calorimetry (DSC) 67
2-3-8 Thermomechanical Analysis (TMA) 68
2-3-9 Universal Testing Machine (UTM) 69
2-3-10 Refractive Index Detector (RI) 70
2-3-11 Ultraviolet–Visible Spectroscopy (UV-Vis) 71
2-3-12 Vector Network Analyzer (VNA) 72
2-3-13 Grazing-Incidence Wide-Angle X-ray Scattering (GIWAXS) 74
2-3-14 Cold Field Emission Scanning Electron Microscope (CFE-SEM) 75
2-3-15 Electrochemical Impedance Spectroscopy (EIS) 77
2-3-16 Vanadium Redox Flow Battery Test (VRFB) 78
2-4 Other Analytical Procedures 80
2-4-1 Water uptake (WU) and Swelling ratio (SR) 80
2-4-2 Ion Exchange Capacity (IEC) 81
2-4-3 Vanadium ion permeability 82
Chapter 3. Results and Discussion: Thermo-Mechanical and Dielectric Optimization of Post-Crosslinked PEI Films for High-Frequency Applications 83
3-1 Synthesis and Crosslinking Design 83
3-2 Film Characterization and Analysis 87
3-3 Thermal and Mechanical Properties of PEIs 92
3-4 Optical Properties of PEIs 97
3-5 Microstructure Analysis via GIXD of PEIs 100
3-6 Dielectric Properties of PEIs 103
3-7 Summary of Low Dielectric Properties Crosslinked PEIs 107
Chapter 4. Results and Discussion: Microphase-Engineered SPI Membranes for Selective Ion Transport in VRFB Systems 110
4-1 Molecular Design and Membrane Fabrication 110
4-2 Film Characterization and Analysis 113
4-3 Thermal and Mechanical Properties 118
4-4 Morphological and Microstructural Characterization 122
4-5 Ion Exchange and Transport Properties 125
4-6 Vanadium Redox Flow Battery Performance 128
4-7 Summary of PI-based PEMs inVRFB 131
Chapter 5. Conclusion and Future Work 133
5-1 Conclusion 133
5-2 Future Work 135
Appendix 136
References 145
                                    

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