臺灣博碩士論文加值系統

由於電子產品的市場對於可攜帶或可穿戴的電子設備的大量需求，使得越來越多研究投入在開發永續性可撓式的能源採集材料。聚偏氟乙烯(PVDF)是具有良好的壓電和熱電性能的材料，它具備高彈性、良好的生物相容性且能夠簡單地大量製備等優勢，使其近年來受到廣泛研究。
PVDF為一半結晶高分子且具有多種結晶相，其中α相為最穩定之結晶相，但其為非極性之結晶結構，不具有壓電及熱電等能力，而具有極性之β結晶相擁有最大壓電和熱電響應之能力，通常藉由機械拉伸或極化方式來獲得β結晶相，要能獲得高壓電及熱電效能之PVDF材料，β結晶相的控制及生長是一極大的關鍵因素。
因此本論文主要區分為三大部分。在第一部分中，探討了球晶微觀結構與β相結晶行為之間的關係，進而理解PVDF的結晶過程及如何控制。透過比較未處理的PVDF薄膜及經極化後的電紡PVDF奈米纖維膜，可以藉由偏光顯微鏡(POM)觀察在電紡PVDF奈米纖維中，有兩種不同球晶同時存在，而與未處理的PVDF薄膜相比，其僅有單一且大顆的球晶，因此證實大顆的球晶為α結晶相，而相對較小及較深的球晶為β結晶相，其甚至嵌入α相之球晶內部，且發現β結晶相的生長速度較α結晶相慢。同時亦透過SEM及AFM之觀察，發現β結晶相成柱狀的結構。最後通過DSC分析和選擇性熔化方法，證明在171 °C的熔融峰歸因於ES誘導的結晶β相的熔化，而在169 °C的峰歸因於α的熔化，澄清PVDF的晶相鑑定。
理解β相的結晶過程後，對於如何提升壓電能力成為一重要參數。因此在論文之第二部分，成功開發一柔性電紡PVDF奈米纖維膜的新型聲能採集裝置，並探討其晶體結構及添加奈米銀 (AgNP) 對PVDF奈米纖維膜的壓電性能之影響。結果顯示，結合靜電紡絲技術和添加AgNP於PVDF中，能有效誘導β相之形成，進而增加了壓電性。然而，藉由PVDF之壓電分流阻尼效應，能將聲音轉成電能，並消耗低頻的聲音傳播，因此在低頻區所產生的電能皆高於中頻及高頻區域，而有添加AgNP的電功率為7×10-4W，相較於沒有添加的PVDF元件 (5×10-4W)，明顯提升了40%。該結果證明PVDF/AgNP具有優異的壓電性能和聲電轉換能力，可有利於運行低功耗的消費電子設備和綠色環境。
而在論文之第三部分，由於太陽能提供了豐富且無處不在的熱能來源，是可再生能源之中的首選，因此將探討PVDF之熱電特性。本章節成功開發一非接觸式光熱轉換制動熱電聚偏氟乙烯之能量擷取器，並藉由添加良好之光熱轉換材料：還原氧化鎢(WO2.72)，增強PVDF/WO2.72奈米纖維膜在近紅外線 (NIR) 區域的吸收能力，同時亦結合部分覆蓋的電極來實現更快及更大的溫度波動，進而強化PVDF的熱電特性。而結果顯示，在NIR照射下，含有7 wt%的PVDF/WO2.72熱電複合材料，其溫度在60秒時，能迅速升至107.1 °C，相較於未含WO2.72的PVDF複合材料高出41.5 °C，且7 wt％的PVDF/WO2.72複合材料之最大輸出電壓可達到1.5 V，相較於未添加WO2.72的PVDF，提升了3倍的電壓輸出，最後在多次的測試循環下，亦證實PVDF/WO2.72複合材料具有良好的熱電能輸出穩定性和耐久性。

The β phase of polyvinylidene fluoride (PVDF) is well known for its piezoelectric and pyroelectric properties and interest for applications in energy harvester. How to obtain a high-level polar β phase of PVDF is an important pursuit.
Thus, this thesis is divided into three parts. In the first chapter, in order to identify the β-phases microstructure, we compared the neat PVDF films and electrospun PVDF nanofibrous membranes. The relationship between spherulitic microstructure and crystallization behavior of the β phase was explored for achieving a proper characterization, understanding and control of the crystallization process. Results showed that the smaller and darker spherulites in electrospun PVDF nanofibrous membranes were implied β phase by polarizing optical microscopy (POM), and even entered inside of the α-phase spherulites. The spherulite growth rate of β phase was lower than the α phase. Meanwhile, the microstructure of β spherulites with a rod-like structure was also observed by SEM and AFM analysis. Then through the DSC analysis and the selective melting method, it proved that the higher melting peak was attributed to the ES-induced melting of the crystalline β phase, whereas the lower peak was attributed to the melting of the α phase. The crystal phase identification for PVDF was clarified.
For the second chapter, a novel sound energy acquisition device based on flexible electrospun PVDF nanofibrous membrane was developed. Effects of the addition of silver nanoparticles (AgNPs) and electrospinning process on the crystal structure and piezoelectric properties of PVDF nanofibrous membranes were examined. Results showed that electrospinning and the addition of AgNP effectively induced β phase formation and increased piezoelectricity. Moreover, the use of piezoelectric shunt damping can reduce the sound transmission at low frequencies. Therefore, electric energy generated in low-frequency region is higher than in mid- and high-frequency regions. Meanwhile, the electric power of PVDF/AgNP is 7 × 10–4 W, which represented a significant increase of 40% compared to PVDF without AgNP (5 × 10–4 W) at low frequency. This result demonstrates that PVDF/AgNP presents excellent piezoelectric properties and acoustic–electric conversion characteristics. It can be beneficial in running low-power consumer electronic devices and green environment.
Then, in the third chapter, the pyroelelctric properties of PVDF was investigated, a novel infrared (IR)-driven non-contact pyroelectric generator based on electrospun PVDF nanofibrous membranes is developed for converting photothermal energy into useful electrical energy. Here, we incorporate a photothermal conversion material: reduced tungsten oxide (WO2.72), into PVDF to enhance the heat transfer of PVDF/WO2.72 nanofibrous membranes, which is due to their excellent IR absorbance. Meanwhile, partially covered electrodes are used to achieve faster and larger temperature fluctuations, which further improve pyroelectric energy transformation. Under IR irradiation, the temperature of the PVDF/WO2.72 pyroelectric composites containing 7 wt% WO2.72 rapidly rises to 107.1 °C after 60 s, which is 41.5 °C higher than that of the WO2.72-free PVDF composites. The maximum output voltage of the WO2.72-free PVDF composites is 0.5 V, while that of the 7 wt% PVDF/WO2.72 composites is three times higher, and reaches 1.5 V. Moreover, the 7wt% PVDF/WO2.72 composites also present good pyroelectric energy output stability and durability.

中文摘要 I
ABSTRACT III
Table of Contents VI
List of Table XI
List of Figures XII
Chapter 1: Introduction 1
1.1 Background 1
1.2 Literature Review 4
1.2.1 Crystallization structure of PVDF 4
1.2.2 Piezoelectric properties of PVDF 7
1.2.3 Acoustic performance 11
1.2.4 Pyroelectric properties of PVDF 14
1.2.5 Photothermal conversion 17
1.2.6 Photothermal conversion material (Tungsten oxide) 20
1.3 Motivation and Objective 23
1.4 Reference 25
Chapter 2: β Phase Crystallization and Melting Behavior of Polyvinylidene Fluoride 38
2.1 Introduction 38
2.2 Experiment 41
2.2.1 Samples preparation 41
2.2.2 Characterization 42
2.3 Results and discussion 43
2.3.1 Crystallization morphology 43
2.3.2 spherulite growth rate 46
2.3.3 Melting behavior 47
2.4 Summary 49
2.5 Reference 50
Chapter 3: Acoustic–Electric Conversion and Piezoelectric Properties of Electrospun Polyvinylidene Fluoride/Silver Nanofibrous Membranes 55
3.1 Introduction 55
3.2 Experiment 59
3.2.1 Materials 59
3.2.2 Preparing electrospun PVDF/AgNP nanofibrous membranes 60
3.2.3 Characterization 61
3.3 Results and discussion 64
3.3.1 Morphology of electrospun PVDF/AgNP nanofibrous membranes 64
3.3.2 Thermal properties of the electrospun PVDF/AgNP nanofibrous membranes 65
3.3.3 Crystallinity of the electrospun PVDF/AgNP nanofibrous membranes 66
3.3.4 Piezoelectricity of the electrospun PVDF/AgNP nanofibrous membranes 70
3.3.5 Sound-absorption coefficient of the electrospun PVDF/AgNP nanofibrous membranes 71
3.3.6 Acoustic electric conversion abilities of the electrospun PVDF/AgNP nanofibrous membranes 74
3.4 Summary 77
3.5 References 78
Chapter 4: Infrared-driven poly(vinylidene difluoride)/tungsten oxide pyroelectric generator for non-contact energy harvesting 85
4.1 Introduction 85
4.2 Experiment 89
4.2.1 Materials 89
4.2.2 Preparation of electrospun PVDF/WO2.72 nanofibrous membranes 90
4.2.3 Preparation of pyroelectric composites using electrospun PVDF/WO2.72 nanofibrous membranes 92
4.2.4 Characterization 93
4.3 Result and discussion 95
4.3.1 Morphology of electrospun PVDF/WO2.72 nanofibrous membranes 95
4.3.2 Crystallinity of electrospun PVDF/WO2.72 nanofibrous membranes 95
4.3.3 Optical and photothermal conversion abilities of electrospun PVDF/WO2.72 nanofibrous membranes 100
4.3.4 Pyroelectricity of electrospun PVDF/WO2.72 nanofibrous membranes 102
4.4 Summary 107
4.5 References 107
Chapter 5: Conclusion 114
Chapter 6: Further Work 116

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