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作者姓名(中文):hardy shuwanto
作者姓名(英文):Hardy Shuwanto
論文名稱(中文):利用大氣電漿一步式製程製備抗菌與導電之自癒合水膠
論文名稱(外文):One Step Preparation of Self-Healing Hydrogels with Antibacterial and Conductive Properties by Atmospheric Pressure Microplasma
指導教授姓名(中文):王孟菊
指導教授姓名(英文):Meng-Jiy Wang
口試委員姓名(中文):魏大欽
吳宗信
蔡大翔
陳賜原
王孟菊
口試委員姓名(英文):Ta-Chin Wei
Jong-Shinn Wu
Dah-Shyang Tsai
Szu-Yuan Chen
Meng-Jiy Wang
學位類別:碩士
校院名稱:國立臺灣科技大學
系所名稱:化學工程系
學號:m10606814
出版年(民國):108
畢業學年度:107
學期:2
語文別:英文
論文頁數:135
中文關鍵詞:自愈水凝膠大氣微電漿導電聚合物物理交聯
外文關鍵詞:self-healing hydrogelsatmospheric pressure microplasmaantibacterialconductive polymerphysical cross-linking
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本論文的研究目標,為利用常壓微電漿製備不同成分與功能的自癒合水凝膠。本論文可分為兩部分: 第一部分為製備銀負載自癒合水凝膠,第二部分為製備具導電性質的自癒合水凝膠。兩種類型的水凝膠都是藉由常壓微電漿掃描丙烯酸 (acrylic acid, AA) 前驅物與氯化鐵 (FeCl 3) 的混合物、藉由添加其他不同的成分而獲得。本論文製備自癒合水凝膠的主要機制,為利用常壓微電漿引起丙烯酸(AA)的聚合反應,並利用氯化鐵做為交聯劑,與聚丙烯酸的羧酸官能團(COO-)和氯化鐵的鐵離子 (Fe 3+) 進行物理交聯,製備自癒合水凝膠。
在添加不同的成份以製備銀負載以及具導電性質自癒合水凝膠之前,先利用水凝膠的機械強度計算自癒合效率,以得到最適化的丙烯酸和氯化鐵混合物的最佳濃度。最適化的結果顯示以 3.5 M丙烯酸與17.5 mM的氯化鐵混合,利用常壓微電漿掃描後的PAA-Fe自癒合水凝膠,可在37°C、12小時間後,顯示 ~68 %、最佳的自癒合效率。將銀顆粒 (Ag) 或明膠 (G)進一步摻入pAA-Fe水凝膠,分別形成pAA-Fe/Ag,pAA-G-Fe和pAA-G-Fe/Ag,SEM圖像顯示在pAA-Fe/Ag可觀察到聚集的氯化銀顆粒 (AgCl),而在pAA-G-Fe/Ag中,由於明膠可有效穩定化氯化銀顆粒,因此觀察到均勻分佈的氯化銀顆粒。XRD分析結晶度證實在水凝膠中的顆粒為銀粒子。僅加入銀粒子的pAA-Fe和pAA-Fe/Ag水膠,在37 ℃下、12小時癒合的自愈效率為~67%,同時,含有銀的兩種水凝膠都對大腸桿菌具有抗菌性,抑制圈的直徑分別為0.92 cm與1.13 cm。另一方面,同時含有銀粒子與明膠的水凝膠,在37 ℃下、12小時癒合時,pAA-G-Fe和pAA-G-Fe/Ag的自癒合效率為~59 %,較低於不含明膠的水凝膠
本論文的第二部分目標為利用經由丙烯酸,氯化鐵和吡咯 (Py) 單體,利用常壓微電漿掃描製備導電自癒合水凝膠。實驗結果顯示,隨吡咯濃度從3.5 mM增加至7.5 mM,pAA-pPY-Fe水凝膠的自愈效率從60.5%下降到32.1 %,此結果與凝膠的含膠率結果一致。此外,利用碘摻雜探討摻雜對於水凝膠導電率的影響,結果顯示碘摻雜可同時提高水凝膠的導電性,以及對大腸桿菌具有較高的抗菌效果。最後,為了證明導電水凝膠的應用,將pAA-pPy7d-Fe與由3V電池供電的LED燈泡連接,形成一個簡單的電路,顯示水凝膠在自癒合過程後可以點亮LED燈泡,證實本研究製備的自癒合水凝膠具有可應用價值。
In this thesis, atmospheric pressure microplasma was employed to prepare self-healing hydrogels with different composition. This thesis is divided into two parts: (part 1): silver loaded self-healing hydrogels, and (part 2): conductive self-healing hydrogels. Both types of the hydrogels were mainly composed by acrylic acid (AA) and ferric chloride (FeCl3). The polymerization of acrylic acid (AA) was proposed to be initiated by the atmospheric pressure microplasma which is postulated to generate free-radicals to initiate radical plasma polymerization. Moreover, the physical cross-linking of hydrogels was facilitated through the carboxylic (COO-) functional groups of polyacrylic acid (pAA) with the added ferric ions (Fe3+) of FeCl3 which resulted in the self-healing hydrogels.
Prior to the syntheses of both types of hydrogels, the optimization of concentrations of AA and FeCl3 was facilitated. The pAA-Fe self-healing hydrogels with concentration of AA 3.5 M and FeCl3 17.5 mM exhibited the optimized self-healing efficiency ~68% for 12 h of healing at 37C.
In the first part, silver loaded self-healing hydrogels were prepared by mixing AA, FeCl3, silver nitrate (AgNO3), and gelatin (G). In this part, four types of hydrogels were synthesized, (1) pAA-Fe, (2) pAA-Fe/Ag, (3) pAA-Fe-G, and (4) pAA-Fe/Ag-G. SEM images revealed that agglomerated silver chloride nanoparticles (AgCl NPs) were observed in pAA-Fe/Ag, whereas in pAA-Fe/Ag-G, AgCl NPs distributed uniformly due to the stabilization of gelatin. The crystallinity of silver in hydrogels was confirmed by XRD analyses which exhibited five diffraction peaks referring to AgCl NPs (JCPDS 31-1238). Furthermore, the self-healing efficiency of gelatin containing hydrogels, pAA-Fe-G and pAA-Fe/Ag-G were found to be ~59%. The hydrogels contained no gelatin, pAA-Fe and pAA-Fe/Ag, revealed the self-healing efficiency of ~67% for 12 hours of healing at 37C. Moreover, the hydrogels containing silver, pAA-Fe/Ag and pAA-Fe/Ag-G, possessed antibacterial activity against E.coli with inhibition zone of 0.92 and 1.13 cm, respectively.
In the second part of this thesis, the conductive self-healing hydrogels composed of AA, FeCl3 and pyrrole monomers were prepared. By atmospheric pressure microplasma treatments, both AA and pyrrole were polymerized to form pAA and polypyrrole (pPy). Herein, the concentration of pyrrole was varied from 3.5 to 7.5 and 10.5 mM namely as pAA-pPy3.5-Fe, pAA-pPy7-Fe and pAA-pPy10.5-Fe, respectively. The decreasing gel fraction was obtained from to 87.5 to 54.5 % with increasing concentration of pyrrole due to pyrrole monomers consumed FeCl3 in the solution forming polypyrrole through oxidative polymerization. The self-healing efficiency of pAA-pPy-Fe hydrogels decreased from 60.5 to 32.1 % with increasing the concentration of pyrrole. This result showed good agreement with gel fraction in which the self-healing efficiency decreased at low gel fraction. Afterward, the effect of undoped and iodine (I2) doped hydrogels were also studied. In this regard, I2 doped hydrogels showed better performance both in antibacterial activity against E.coli bacteria and conductivity by four-point probe method compared to undoped hydrogels. Finally, as representative, pAA-pPy7d-Fe was chosen considering its self-healing efficiency and conductivity for the evaluation of electrical conductivity applications in a simple electrical circuit which was powered by 3 V batteries. Briefly, the initial hydrogel and after-healed hydrogel were able to conduct electricity indicated by lighting-up the LED in the electrical circuit.
Content of Thesis

摘 要 2
Abstract 4
Acknowledgement 6
Content of Thesis 7
List of Figures 10
List of Tables 15
Chapter 1. Introduction 16
Chapter 2. Literature review 19
2.1. Self-healing materials 19
2.2. Self-healing hydrogel 20
2.2.1. Dynamic covalent bonding 21
2.2.2. Non-covalent interactions 23
2.3. Free radical polymerization 24
2.4. Plasma technology 25
2.4.1. Atmospheric pressure plasmas 27
2.4.2. Non-atmospheric plasmas 28
2.4.3. Local thermodynamic (thermal) equilibrium plasmas 29
2.4.4. Non-local thermodynamic equilibrium plasmas 29
2.5. Acrylic acid 32
2.6. Silver nanoparticles 33
2.7. Gelatin 35
2.8. Polypyrrole 37
Chapter 3. Experimental 39
3.1. Chemicals 39
3.1.1. Preparation of hydrogels 39
3.1.2. Antibacterial experiments 40
3.2. Equipment and instruments 40
3.3. Experimental procedures 41
3.3.1. [A] Optimization of concentrations of AA and FeCl3 41
3.3.1. [B] Optimization of concentrations of silver 42
3.3.1. [C] Optimization of concentrations of gelatin 43
3.3.2. Preparation of silver loaded self-healing hydrogels 44
3.3.3. Preparation of conductive self-healing hydrogels 45
3.4. Analyses and characterizations 46
3.4.2. Optimization of concentrations of AA and FeCl3 47
3.4.3. Silver loaded self-healing hydrogels 52
3.4.4. Conductive self-healing hydrogels 56
Chapter 4. Results and Discussion 60
4.1 OES analyses 60
4.2. Preparation of pAA-Fe and silver and/or gelatin containing self-healing hydrogels 61
4.2.1 Optimization of concentrations of AA and FeCl3 for pAA-Fe hydrogels 61
4.2.1 [A] Effects of concentrations of AA and FeCl3 on swelling degree and gel fraction 61
4.2.1 [B] GPC analyses 63
4.2.1 [C] Effects of concentrations of AA and FeCl3 on self-healing efficiency 63
4.2.1 [D] Effects of time of healing and temperatures of healing on self-healing 65
4.2.1 [E] Effects of concentrations of silver on swelling degree and gel fraction 67
4.2.1 [F] ICP analyses 67
4.2.1 [G] Effect of silver concentration on antibacterial activity 67
4.2.1 [H] Effect of concentration of gelatin on degree of swelling and gel fraction 68
4.2.1 [I] Effect of concentration of gelatin on self-healing efficiency 68
4.2.1 [J] Effect of concentration of gelatin on surface morphology 69
4.2.2. Silver-loaded and/or gelatin incorporated self-healing hydrogels 70
4.2.2 [A] Chemical functionalities by FTIR analyses 70
4.2.2 [B] SEM and EDX analyses 71
4.1.2 [C] XRD analyses 71
4.2.2 [D] Equilibrium degree of swelling and gel fraction 72
4.2.2 [E] Self-healing efficiency 72
4.2.2 [F] Antibacterial activity 73
4.3. Conductive self-healing hydrogels 73
4.3.1. Chemical functionalities by FTIR analysis for conductive self-healing hydrogels 73
4.3.2. Equilibrium degree of swelling and gel for conductive self-healing hydrogels 74
4.3.3. Self-healing efficiency for conductive self-healing hydrogels 74
4.3.4. Antibacterial activity for conductive self-healing hydrogels 75
4.3.5. Conductivity of self-healing hydrogels measured by four-point probe methods 76
4.3.6. The applications of conductive self-healing hydrogels 76
Chapter 5. Conclusions 106
References 109
Appendix: Q & A 126

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