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研究生： 賴柏丞
Lai, Po-Cheng
論文名稱： 以纖維素奈米晶體為基底製備可直接書寫式列印之離子凝膠及其於穿戴式感測器之應用
Direct ink writing of ionic gels based on cellulose nanocrystals for wearable sensor
指導教授： 游聲盛
Yu, Sheng-Sheng
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： 2022
畢業學年度： 110
語文別： 英文
論文頁數： 107
中文關鍵詞： 3D 列印 、水凝膠 、纖維素奈米結晶 、深共熔溶劑 、離子凝膠 、穿戴式感測器
外文關鍵詞： 3D printing, nanocomposite hydrogels, cellulose nanocrystals, stretchable electronics, deep eutectic solvents, nanocomposite ionogels, wearable sensors
相關次數： 點閱：149  下載：9 
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    • 近年來由離子凝膠材料已被陸續應用於可穿戴式電子裝備及人造肌肉的領域，離子凝膠通常由可自由移動的離子及聚合物網絡所構成，並具備良好的離子導電性。上述應用通常要求凝膠堅韌、透明且可3D列印。另一方面，永續性材料的利用，也是現今研究循環經濟的主要課題。在眾多生物質材料中，纖維素奈米結晶 (Cellulose nanocrystals, CNCs)具備特殊的機械性質及流變性質，且由於其表面帶有許多羥基，可進行多種表面修飾。本研究分別以不同的概念設計了兩款具備不同性質的直接書寫式3D列印 (Direct ink writing)墨水，並將其應用於穿戴式人體感測器。
    首先，我們設計了一種結合陽離子型纖維素奈米晶體 (Cationic cellulose nanocrystals)及兩性離子單體的水凝膠墨水。CCNCs首先被分散在單體的水溶液中，以製備具有動態物理網絡的墨水，利用UV光聚合及額外引入鋁離子的方式製備了含有多重物理交聯的水凝膠材料。與使用傳統 CNCs 的水凝膠相比，CCNCs在水中能與聚合物網絡形成更有效的鍵結，能夠顯著改變水凝膠之流變及機械性質，並降低3D列印所需的奈米材料用量。
    另外，由於水凝膠材料經常受到水分蒸發的影響，我們以深共熔溶劑 (Deep eutectic solvent, DES)及CNCs製備出新型離子凝膠，並用於直接書寫式3D列印及可自癒合之穿戴式感測器。我們發現可透過簡單的加熱製程誘導CNCs在低濃度下，形成可3D列印之凝膠墨水。我們選擇丙烯酸（Acrylic acid, AA）和丙烯醯胺（Acrylamide, AAm）構建強韌的聚合物網絡。並進一步引入鋁離子與聚丙烯酸單元產生進一步物理交聯。此CNCs/DES離子凝膠具備高韌性及可拉伸性，且由於高分子網絡與DES間有充足的動態物理鍵結，如氫鍵作用力及離子鍵結，此離子凝膠能夠在發生斷裂時自我修復，展現材料的自癒合性質。
    在這兩項策略中，我們分別改變了CNCs的表面化學和CNCs於DES中的分散製程，成功減少了水凝膠和離子凝膠中的奈米粒子用量，以實現更高的透明度及良好的自修復性質。以CCNCs為基底的水凝膠和以 CNCs/DES為基底的離子凝膠可分別組裝為電容型感測器及電阻型感測器。3D 列印使得我們能進一步製備具特殊設計的感測器，並提高其靈敏度。透過改變納米晶體的表面化學及改善分散製程，我們的奈米複合水凝膠和離子凝膠展現了多功能性，包括良好的機械強度、高透明度、自修復能力和可3D列印性

    Ionogels are soft materials that have been applied in wearable electronic and artificial muscles. These applications often require the ionogels to be tough, transparent, and 3D printable. Renewable materials like cellulose nanocrystals (CNCs) with tunable surface chemistry provide a way to prepare tough nanocomposite ionogels. Here, we designed ink for 3D printable sensors with two different concepts.
    First, we design an ink with cationic cellulose nanocrystals (CCNCs) and zwitterionic hydrogels. CCNCs were first dispersed in an aqueous solution of monomers to prepare the ink with a reversible physical network. Subsequent photopolymerization and the introduction of Al3+ ion led to strong hydrogels with multiple physical cross-links. Compared to the hydrogels using conventional CNCs, CCNCs formed a stronger physical network in water that greatly reduced the concentration of nanocrystals needed for reinforcing and 3D printing.
    Second, we utilized deep eutectic solvents (DES) as alternative solvents to prepare 3D printable and self-healable ionogels with low volatility and overcome low stability of common hydrogels due to the evaporation of water. By simply heating the dispersion of CNCs/DES, the gelation of CNCs could be effectively induced. Acrylic acid (AA) and acrylamide (AAm) were chosen to construct a single network copolymer system under photopolymerization. The introduction of Al3+ ions provided additional physically cross-linking. With abundant dynamic physical bonds such as hydrogen bonding and ionic interactions between the polymer chains and DES, the ionogels could self-heal after a fracture.
    In short, we presented two strategies to reduce the content of nanoparticles in hydrogels and ionogels to achieve high transparency and simple dispersion. CCNCs based hydrogels and CNCs/DES based ionogels were assembled as capacitive sensor and resistive sensor, respectively. 3D printing further enabled a facile design of tactile and special pattern sensors with enhanced sensitivity. By harnessing the surface chemistry of the nanocrystals, our nanocomposite hydrogels and ionogels achieved multifunctionality containing good mechanical strength, high transparency, self-healing ability, and 3D printability.

    Abstract I TABLE OF CONTENTS V LIST OF FIGURES IX LIST OF TABLES XVIII CHAPTER 1. Introduction 1 1.1 Hydrogel 1 1.1.1 Introduction of hydrogel 1 1.1.2 Design of hydrogels 2 1.1.3 Hydrogel ionotronics 4 1.2 3D printing 6 1.2.1 Introduction of 3D printing 6 1.2.2 Fused deposition modeling (FDM) 7 1.2.3 Stereolithography (SLA) 8 1.2.4 Digital light processing (DLP) 9 1.2.5 Direct ink writing (DIW) 10 1.3 Cellulose nanocrystals (CNCs) 12 1.3.1 Introduction of CNCs 12 1.3.2 Properties of CNCs 12 1.3.3 Modification of CNCs 13 1.4 Deep eutectic solvent (DES) 15 1.4.1 Introduction of DES 15 1.4.2 Types of DES 16 1.4.3 Properties of DES 17 1.4.4 Application of DES 18 1.5 Objective 20 Chapter 2. Cationic cellulose nanocrystals nanocomposite hydrogels 21 2.1 Objective 21 2.2. Experimental methods 23 2.2.1 Materials 23 2.2.2 Synthesis of CCNCs 23 2.2.3 Preparation of the CCNCs nanocomposite gels 24 2.2.4 Rheological analysis 24 2.2.5 Mechanical test 25 2.2.6 3D printing 25 2.2.7 Electrical measurement 26 2.2.8 Characterization 27 2.3 Results and discussion 28 2.3.1 Rheological behavior of the CCNCs dispersion in water 28 2.3.2 Mechanical property of the CCNCs nanocomposite hydrogels 34 2.3.3 Self-recovery properties of the CCNCs nanocomposite hydrogel. 40 2.3.4 Ionic conductivity of the CCNCs nanocomposite hydrogels 47 2.3.5 CCNCs nanocomposite hydrogels for 3D printing and wearable sensors 48 2.3.6 Discussion 55 2.3.7 Conclusion 55 CHAPTER 3. CNC/DES nanocomposite ionogels 57 3.1 Objective 57 3.2 Experimental methods 58 3.2.1 Materials 58 3.2.2 Preparation of Ionogels 59 3.2.3 Rheological analysis 60 3.2.4 Mechanical and self-healing test 60 3.2.5 3D printing 60 3.2.6 Electrical measurement 61 3.2.7 Characterization 62 3.3 Results and discussion 63 3.3.1 Rheological behavior of the CNCs/DES nanocomposite ink 63 3.3.2 Mechanical properties of CNCs/DES nanocomposite ionogels 69 3.3.3 Self-healing property of nanocomposite ionogels 79 3.3.4 Ionic conductivity of CNCs/DES nanocomposite ionogels 81 3.3.5 Demonstration of 3D printing and potential application of ionogels 82 3.3.6. Discussion 87 3.3.7. Conclusion 88 CHAPTER 4. References 89

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