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輔仁大學
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詹智傑
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Chih-Chieh Chan
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以靜電紡絲技術製備聚乙烯醇 / 石墨烯奈米纖維
PVA/Graphene Electrospun Nanofibers Prepared by Electrospinning Technique
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Yuan-Hsiang Yu

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摘要 目錄
第五章
第一章
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緒論 第二章 實驗部分 第三章 結果與討論 第四章
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聚乙烯醇 石墨烯 靜電紡絲 奈米纖維
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Poly(vinyl alcohol) Graphene electrospinning nanofiber
摘要
( 中 )
本論文使用改良的 Hummers’ method 將石墨氧化成氧化石墨烯 (Graphene oxide, GO) ，之後再進一步以甘氨酸 (Glycine) 還原修飾 GO 得到官能基化
的氧化石墨烯 (Functionalized graphene oxide, FGO) ，最後以水相的溶液分
散法 (Solution dispersion) 製備出一系列的官能基化石墨烯 (FGO)/ 聚乙烯醇
(Poly(vinyl alcohol), PVA) 奈米複合材料，並以靜電紡絲設備經由不同條件
( 電壓、幫浦流速、針頭至收集板之距離、高分子濃度， FGO 濃度 ) 來控
制奈米纖維的直徑與形態。 FGO 的鑑定以及靜電紡絲的結構則透過穿透
式電子顯微鏡 (TEM) 、掃描式電子顯微鏡 (SEM) 、熱失重分析儀 (TGA) 、
化學分析影像能譜儀 (XPS) 、微差掃描式熱分析儀 (DSC) 、廣角 X-ray 繞

射儀 (XRD) 進行分析。從 SEM 圖可發現奈米纖維的形貌會因為添加少量
FGO 而獲得改善 (0.1~0.5 wt %) ，實驗中得知 FGO 只需添加 0.5 % 就可明
顯增加 PVA 之熱穩定性，如在 TGA 圖中， 0.5 % FGO/PVA 相較於純
PVA 纖維，熱裂解溫度 (Td) 提高約 20 ℃， DSC 圖中也看到玻璃轉換溫度
(Tg) 增加約 3 ℃，而當 FGO 添加過多，性質也不會有太大改變甚至因為
分散性不佳而使材料性質變差。最後我們利用 FGO 與 HAuCl4 反應，使
奈米金 (Nanogold) 生長於石墨層之表面 ( 稱之為 FGO-Au) ，而同樣添加至
PVA 之中，形成 FGO-Au/PVA 溶液，並製備成奈米纖維，再以阻抗頻譜
分析儀測量纖維的電性質，發現僅添加 0.3 % FGO-Au 至 PVA 中，其阻
抗明顯減少，而得知 FGO-Au 可以提升 PVA 纖維的導電性，預期未來可
應用於感應器領域。
摘要
( 英 )
論文
目次
A series of poly (vinyl alcohol) (PVA)/functionalized graphene oxide (FGO) nanofibers with low feeding ratios of FGO to PVA were fabricated by electrospinning method. In this study, the prepared PVA/FGO nanocomposites were dispersed in water phase followed by electrospinning treatment under different operational parameters (i.e., applied voltage, feeding rate and FGO contents) to give nanofibers of various diameters and morphologies. The morphology, diameter and structure of electrospun nanofibers and FGO were investigated by Fourier transform infrared (FT-IR) spectroscopy, X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD) and differential scanning calorimetry (DSC). SEM images showed that the morphologies of the nanofibers were improved by the incorporation of FGO at a low loading content (e.g., 0.1~0.5 wt %) as compared to pure electrospun PVA.
The thermal stability of PVA/FGO nanofibers were also studied. Experimental results indicated that the thermal stability of PVA fibers can be significantly increased by simply incorporation with 0.5 % FGO, such as TGA curves showed that the thermal decomposition temperature (Td) was increase about 20 ℃ for the
0.5 % FGO/PVA compared to the pure PVA fibers. DSC curves also see the glass transition temperature (Tg) increased about 3 ℃ . However, if FGO added too much, the material properties will not be much changed, and even worse because of poor dispersion. Finally, gold nanoparticles were successfully fabricated on the surface of FGO-Au by reducing of HAuCl4. And the same, nanofibers with low feeding ratios of FGO-Au to PVA were fabricated by electrospinning method.
Electrochemical impedance spectrum (EIS) analyses in the electrical properties of the as-prepared fibers, found that only 0.3 % FGO-Au added to the PVA, could significantly reduce the impedance. Therefore, FGO-Au could be used to improve the conductivity of the PVA fibers, which is expected to be applied to the sensor fields.
目錄 摘要 I Abstract II 目錄 IV 圖目錄 VII 表目錄 XIII 第一章 緒論 1 1-1
前言 1 1-2 石墨烯介紹及製備 4 1-2-1 石墨烯之簡介 4 1-2-2 石墨烯的化學
與物理性質 6 1-2-3 石墨烯的合成 7 1-2-4 石墨烯之鑑定 11 1-2-5 石墨烯之
應用 18 1-3 聚乙烯醇 /Graphene 奈米複合材料之介紹 20 1-3-1 聚乙烯醇

(Poly(vinyl alcohol) ， PVA) 之介紹 20 1-3-2 奈米複合材料之種類 22 1-3-3
PVA/graphene 奈米複合材料之介紹 24 1-4 靜電紡絲 (electrospun) 之介紹 27
1-4-1 簡介 27 1-4-2 靜電紡絲裝置 27 1-4-3 靜電紡絲原理 28 1-5 PVA 靜電
紡絲纖維之文獻回顧 30 1-6 研究動機 36 第二章 實驗部分 38 2-1 實驗藥
品 38 2-2 儀器 40 2-2-1 實驗儀器 40 2-2-2 分析儀器 42 2-3 實驗步驟 44 2-
3-1 Improved Hummers’ method 製備氧化石墨烯之合成 44 2-3-2 氧化石墨
烯之改質 : FGO 之合成 46 2-3-3 FGO 改質成 FGO-Au 之合成方法 48 2-3-4
溶液分散法製備 FGO/PVA 奈米複合材料之溶液 50 2-3-5 FGO/PVA 以靜
電紡絲技術製備奈米纖維 52 2-3-6 FGO/PVA 靜電紡絲薄膜之製備方式 53
2-3-7 FGO-Au/PVA 以靜電紡絲技術製備工作電極 54 第三章 結果與討論
55 3-1 FGO 之傅立葉轉換紅外線光譜儀 (FTIR) 鑑定 55 3-2 FGO 之化學分
析電子光譜儀 (XPS) 鑑定 58 3-3 FGO 之熱失重分析儀 (TGA) 鑑定 62 3-4
FGO 之掃描式電子顯微鏡 (SEM) 之鑑定 64 3-5 FGO 之穿透式電子顯微鏡
(TEM) 之鑑定 69 3-6 FGO 之廣角 X-Ray 繞射儀 (XRD) 鑑定 72 3-7 FGO 之
拉曼光譜 (Raman spectroscopy) 鑑定 74 3-8 SEM 鑑定聚乙烯醇靜電紡絲纖
維 76 3-8-1 高分子濃度對靜電紡絲纖維型態之影響 76 3-8-2 幫浦流速對
靜電紡絲纖維型態之影響 78 3-8-3 電壓對靜電紡絲纖維型態之影響 80 3-
9 SEM 鑑定 FGO/PVA 靜電紡絲纖維 82 3-9-1 不同比例 FGO 對 PVA 靜電
紡絲纖維型態之影響 82 3-9-2 電壓對 FGO/PVA 靜電紡絲纖維型態之影響
84 3-9-3 幫浦流速對 FGO/PVA 靜電紡絲纖維之影響 86 3-10 FGO/PVA 靜
電紡絲纖維之鑑定 87 3-10-1 穿透式電子顯微鏡 (TEM) 觀察 FGO/PVA 奈米
纖維之形貌 87 3-10-2 X-Ray 繞射儀之鑑定 FGO/PVA 奈米纖維 88 3-10-3
熱失重分析儀 (TGA) 分析奈米纖維之熱性質 90 3-10-4 微差掃描式熱分析
儀 (DSC) 分析奈米纖維之熱性質 92 3-10-5 DMA 分析奈米纖維之機械性質
94 3-10-6 萬能拉力機測試奈米纖維之機械性質 95 3-10-7 電化學分析奈米
纖維之電性質 96 第四章 結論 98 第五章 參考文獻 99
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