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研究生： 黃建豪
Chien-Hao Huang
論文名稱： 以電紡技術製備用於燃料電池觸媒層之白金奈米纖維
The Preparation of Pt-Catalyst Layer for Fuel Cells by Using the Electrospinning
指導教授： 何明樺
Ming-Hua Ho
口試委員: 張敏興
Min-Hsing Chang
白孟宜
Meng-Yi Bai
學位類別： 碩士
Master
系所名稱： 工程學院 - 化學工程系
Department of Chemical Engineering
論文出版年： 2011
畢業學年度： 99
語文別： 中文
論文頁數： 132
中文關鍵詞： 電紡 、PVP 、白金纖維 、交聯程序
外文關鍵詞： electrospinning, PVP, Pt fibers, cross-linking process
相關次數： 點閱：283  下載：18 
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  •  上一筆

    • 本實驗利用靜電紡絲法製備高分子PVP與白金前驅物所合成之複合奈米纖維，再以高溫移除高分子與還原白金前驅物形成具有高電導度與高比表面積之白金金屬奈米纖維，探討燒結後的金屬纖維之型態、元素組成、電化學性質與電性等最佳化研究，並且使用各種方法如降低燒結速率、中間層塗布、碳基材表面改質與交聯程序等進行煅燒程序後白金纖維薄膜均勻化之探討，期待作為質子交換膜燃料電池中陽極觸媒層的應用。
    首先進行白金奈米纖維最佳化之製備，包含材料參數如高分子PVP濃度、溶劑之間的比例與白金前驅物濃度和電紡操作參數如電壓大小、流率大小以及雙極間距等最佳化程序。再煅燒後，以FESEM分析纖維型態及尺寸，可得尺寸40nm大小之奈米纖維，大幅提高比表面積。使用四點碳針儀進行電導度測試，可達3×104 S/cm之高電導度值，提高電子在電觸媒層上傳輸的速率。
    在薄膜均勻化部份，將高分子白金纖維沉積在碳紙擴散層後，使用Glutaraldehyde(GA)作為交聯劑交聯高分子鏈形成網狀結構，在燒結過成中能抑制纖維的收縮達到薄膜均勻貼附的效果，增加電池大小的可能性，實現以金屬纖維作為質子交換膜燃料電池電觸媒層之
    發展性。

    The electrospun Pt nanofibers are prepared by the electrospinning of PVP-Pt solution, and then the PVP is removed by calcination in the air. The PVP concentration, solvent composition, Pt concentration, flow rate, applied voltage and discharging distance in the electrospinning are all optimized in this study. After that, the calcinations temperature and period are also investigated. To analyze the structure and properties of metallic nanofibers, SEM, TEM and EDS were applied to obtain the morphologyof nanofibers and the distribution of Pt in fibers. The Pt-fibrous layer are homogenized by several methods, including decrease of heating rate，coating of middle layer，surface modification for carbon support and cross-linking process.
    The results indicated that the Pt nanofibers fabricated in this research are highly alloyed. With the optimized conditions in the electrospinning process, the diameters of nanofibers were smaller than 40 nm and with homogeneous distribution of Pt. The results also show a higher electrical conductivity of Pt nanofibers, compared with those of the conventional Pt nanoparticle catalysts. By using the pre-crosslinking with GA vapor and the post-crosslinking with concentrated GA solution, the shrinkage caused by calcinatiion can be avoided. Thus, a homogeneous catalyst layer composed of Pt electrospun fibers is successfully prepared in this study. The adhesion between carbon paper and Pt-fibrous catalyst layer is good in a large area. The enhancements of electrocatalytic properties for the Pt nanofibers could outperform on the electro-oxidations over the fuel cell electrodes.

    中文摘要 I 英文摘要 II 致謝 III 目錄 IV 圖目錄 VIII 表目錄 XVI 第一章 序論…...…...…...……………………………………… ……..1 第二章 文獻回顧 2.1 質子交換膜燃料電池 4 2.1.1 發展史 4 2.1.2 工作原理與電池結構 5 2.1.3 薄膜電極組 8 2.1.3.1 高分子薄膜 8 2.1.3.2 電極 10 2.1.3.2-1 三相界面 11 2.1.3.2-2 氣體擴散層 14 2.1.3.2-3 電催化層 15 2.1.4 流場版 16 2.1.5 電催化層 16 2.1.5.1 陽極電催化層 16 2.1.5.2 陰極電催化層 17 2.1.5.3 載體 17 2.1.5.3-1 碳粉 18 2.1.5.3-2 石墨纖維 18 2.1.5.3-3 奈米碳管 29 2.1.5.3-4 多孔碳 20 2.1.5.3-5 奈米突 21 2.1.5.3-6 奈米纖維 22 2.1.5.3-7 導電高分子 25 2.1.5.4 白金觸媒沉積到碳載體上的製備 25 2.2 載體金屬奈米纖維(Supported metal Nanofibers) 25 2.3 以靜電紡絲技術製備奈米金屬線 27 2.3.1 靜電紡絲(electrostatic spinning) 28 2.3.2 影響靜電紡絲的因素 30 2.3.3 不穩定性 31 2.3.4以靜電紡絲製備無機奈米纖維材料及在燃料電池的應用 35 第三章 實驗 3.1 實驗材料與藥品 42 3.2 實驗設備 44 3.2.1 靜電紡絲系統 44 3.2.2 箱型程控高溫爐 44 3.2.3 精密式電磁加熱攪拌器 44 3.3 分析儀器 45 3.3.1 掃描式電子顯微鏡(Scanning Electron Microscope, SEM) 45 3.3.2 X光能譜散佈分析儀(Energy Dispersive Spectrometer, EDS) 45 3.3.3穿透式電子顯微鏡(Transmission Electron Microscope,TEM)46 3.3.4 四點探針薄膜測量儀(Four Point Probe) 47 3.3.5 電化學分析法-循環伏安法(cyclic voltametry) 47 3.3.6 熱重分析儀(Thermogravimetry Analyzer, TGA) 52 3.4 實驗方法 52 3.4.1 高分子與白金前驅物混合溶液配製 52 3.4.2 電紡程序 52 3.4.3 預交聯程序 53 3.4.4 後交聯程序 53 3.4.5 煅燒處理 54 3.4.6 碳基材表面改質 54 3.5 試片分析 54 3.5.1 SEM表面影像分析 54 3.5.2 EDS元素分析 55 3.5.3 TGA熱重分析 55 3.5.4 TEM結構分析 56 3.5.5 循環伏安法燃料測試 56 3.6 實驗流程圖 57 第四章 實驗結果與討論 4.1 以靜電紡絲製備高分子PVP白金纖維(PVP-Pt fibers) 59 4.1.1 高分子濃度對高分子白金纖維型態的影響 59 4.1.2 溶劑比例對於高分子白金纖維型態的影響 63 4.1.3 白金前驅物的濃度對高分子白金纖維型態的影響 66 4.1.4 靜電紡絲機之輸出電壓對高分子白金纖維的影響 69 4.1.5 流率對高分子白金纖維的影響 71 4.1.6 靜電紡絲機之雙極間距對高分子白金纖維的影響 73 4.2 以煅燒程序移除高分子製備白金纖維(Pt fibers) 76 4.3 電觸媒層白金纖維薄膜之均勻化探討 86 4.3.1 降低到達高分子移除溫度的升溫速率 88 4.3.2 使用中間層(sublayer)作為黏著層 90 4.3.3 使用電漿處理(plasma treatment)進行碳基材表面改質 93 4.3.3.1 以O2電漿進行碳紙表面親水處理 94 4.3.3.2 以Ar電漿進行碳基材表面粗糙度改質之蝕刻處理 96 4.3.4 使用交聯程序抑制纖維薄膜收縮問題 102 4.3.4.1 前交聯處理 103 4.3.4.2 後交聯處理(Post Crosslinking) 109 4.3.4.3 預交聯處理(Pre- Crosslinking) 113 4.4 白金纖維薄膜電極之電化學活性分析 119 第五章 結論 121 參考文獻 122

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