以奈米級碳材料作為染料敏化太陽能電池對電極之研究

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研究生：	許家彰 Hsu, Chia-Chang
論文名稱：	以奈米級碳材料作為染料敏化太陽能電池對電極之研究 Investigations on the Application of Nanoscale Carbon Materials as Counter Electrodes of the Dye-Sensitized Solar Cells
指導教授：	戴念華 Tai, Hyan-Hwa 李紫原 Lee, Chi-Young
口試委員:
學位類別：	碩士 Master
系所名稱：	工學院 - 材料科學工程學系 Materials Science and Engineering
論文出版年：	2009
畢業學年度：	97
語文別：	中文
論文頁數：	124
中文關鍵詞：	染料敏化太陽能電池、對電極、碳材料、催化
外文關鍵詞：	dye-sensitized solar cells, counter electrodes, carbon materials, catalysis
相關次數：	點閱：2 下載：0
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本研究利用奈米級碳材料作為染料敏化太陽能電池之對電極，藉由交流阻抗、循環伏安法、穩態伏安法與光電轉換特性等方法，研究各式碳極對碘離子/三碘錯離子氧化還原對之還原能力。實驗結果發現，碳極的表面積會強烈影響介面電荷轉移阻抗、I3－離子還原效率與光電轉換效率。由電子轉移控制與質傳控制之互動關係得知，奈米碳粉電極具有催化電解液能力，而多壁奈米碳管電極和少壁奈米碳管電極僅為輔助催化電解液，藉由分析奈米碳粉/少壁奈米碳管複合電極特性得知，奈米碳粉電極催化電解液能力不及鉑金屬。
本研究使用熱沉積鉑金屬為對電極，所得的光電轉換效率為4.136 %，以少壁奈米碳管電極作為對電極其光電轉換效率為3.156 %。由此結果可推論，奈米碳材料有機會取代鉑金屬作為染料敏化太陽能之對電極。使用鉑/少壁奈米碳管復合電極，以鉑金屬顆粒作為催化活躍位置，藉由少壁奈米碳管的高表面積，提升光電轉換效率。
最後，本研究提出一套完整的對電極分析方法與流程，並且探討碳材料的結構、表面形貌、表面積與缺陷等因素對電極的導電性、催化活性與穩定性的關係，並提出碳材料應用於染料敏化太陽能電池對電極的準則。

We utilize nanoscale carbon materials as the counter electrodes of dye-sensitized solar cells (DSSCs) to explore how the catalytic ability of carbon electrodes responds to iodium/triiodide redox. We find that the surface area of carbon electrodes has markedly influences on the charge transfer resistance, the efficiency of catalytic process of I3－ ions, and the energy conversion efficiency. Through the relationship between charge transfer and mass transfer control, nanocarbon electrodes possess the ability to catalyze electrolyte; on the other hand, both MWNTs and LWNTs only play the role of assistance. Moreover, according to the experimental result, the catalytic ability of nanocarbon electrodes is inferior to the Pt electrode.
The energy conversion efficiency of thermal deposited Pt and LWNTs counter electrodes are 4.136 % and 3.156 %, respectively, which indicates that LWNTs has the potential to substitute Pt as counter electrodes of DSSCs. This energy conversion efficiency of the Pt/LWNTs electrode can be enhanced due to increasing surface areas of LWNTs and employing Pt particles as the active sites of catalysis.
This work proposes a thorough method to analyze counter electrode and shows how the parameters such as structure, morphology, surface areas, and defects of materials, affect the electric conductivity, catalytic activity, and stability of the electrode. Furthermore, this study also establishes a criterion for the application of carbon materials as counter electrode in DSSCs.

總目錄
摘要………………………………………………………………………I
Abstract…………………………………………………………………II
致謝……………………………………………………………………III
總目錄 …………………………………………………………………IV
圖目錄…………………………………………………………………VIII
表目錄 ………………………………………………………………XIII
第一章    緒論……………………………………………………………1
1.1 前言………………………………………………………………1
1.2 太陽能電池簡介…………………………………………………2
1.3 染料敏化太陽能電池(Dye-Sensitized Solar Cells, DSSC)………4
1.4 研究動機…………………………………………………………5
第二章    文獻回顧與理論基礎……………………………………………7
    2.1染料敏化太陽能電池工作原理…………………………………7
2.2染料敏化電池各層組成探討……………………………………8
2.2.1 二氧化鈦陽極電極…………………………………………8
2.2.2表面修飾染劑……………………………………………10
2.2.3 電解質溶液………………………………………………11　
2.2.4 相對電極(陰極)………………………………………13
2.3 太陽能電流電壓輸出特性………………………………………15
2.4 交流阻抗原理與模擬等效電路…………………………………16
2.4.1交流阻抗原理………………………………………………16
  2.4.2太陽能電池之模擬等效電路………………………………19
2.5 電極反應動力學理論…………………………………………21
2.5.1極化………………………………………………………21
2.5.2電極反應動力學…………………………………………22
2.6 奈米碳管的起源、結構與製備………………………………23
2.6.1奈米碳管的起源…………………………………………23
2.6.2奈米碳管的結構…………………………………………23
2.6.3水平流動觸媒化學沉積法製備奈米碳管………………24
第三章    研究方法與實驗步驟……………………………………………34
3.1實驗藥品與實驗儀器…………………………………………34
3.2 實驗步驟……………………………………………………37
3.2.1碳管材料製備………………………………………………37
  3.2.1.1水平式懸浮觸媒化學氣相沉積法…………………37
  3.2.1.2多壁奈米碳管實驗成長步驟………………………38
  3.2.1.3多壁奈米碳管粉末之純化…………………………39
3.2.2電極製作…………………………………………………40
3.2.3電池組裝…………………………………………………42
3.3 量測儀器使用方式………………………………………………43
3.3.1光電轉換特性量測…………………………………………43
3.3.2全電池光源下電化學阻抗光譜分析………………………43
3.3.3碳極電荷轉移阻抗分析……………………………………44
3.3.4循環伏安法(Cyclic Voltammetry)…………………………44
3.3.5穩態伏安法(Steady-State Voltammetry)……………………45
第四章    結果與討論………………………………………………………50
4.1 製程之優化………………………………………………………50
4.1.1導電玻璃穿透度與電阻之影響……………………………50
4.1.2鉑金屬對電極製程方法之影響……………………………51
4.1.3電解液溶劑之影響…………………………………………53
4.1.4電解質DMPII添加對染料敏化太陽能電池之影響……54
4.2各式碳極(nano carbon, MWNTs, LWNTs)特性之比較…………56
4.2.1各式碳極之BET、BJH與SEM表面形貌分析…………56
4.2.2各式碳極之電性分析……………………………………57
4.2.3各式碳極之光電轉換效率與全電池EIS分析…………58
4.2.4各式碳極之電荷轉移阻抗分析……………………………60
4.2.5各式碳極之循環伏安法(Cyclic Voltammetry, CV)分析…62
4.2.6各式碳極之穩態伏安法(Steady-State Voltammetry)分析…64
4.2.7各式碳極材料粉末結構……………………………………66
4.3 Pt/LWNTs電極作為DSSC對電極之影響………………………69
  4.3.1 Pt/LWNTs電極之製程改變與SEM表面形貌……………69
      4.3.2 Pt/LWNTs電極光電轉換效率與全電池EIS分析………69
4.4 nano carbon/LWNTs電極作為DSSC對電極之影響……………72
  4.4.1 nano carbon/LWNTs電極之製程改變與SEM表面形貌…72
      4.4.2 nano carbon/LWNTs電極光電轉換效率與全電池EIS分析73
      4.4.3 碳材料作為染料敏化太陽能電池對電極之準則…………74
第五章    結論與建議……………………………………………………105
5.1 結論……………………………………………………………105
5.2 建議……………………………………………………………107
參考文獻…………………………………………………………………109
附錄A……………………………………………………………………118

圖目錄

圖1-1 現今能源使用比例…………………………………………………6
圖2-1 染料敏化電池理論工作原理圖…………………………………26
圖2-2 染料敏化電池實際工作原理圖…………………………………26
圖2-3 染料敏化太陽能電池結構圖……………………………………27
圖2-4 染劑對TiO2及電解液能階示意圖………………………………27
圖2-5 (a)N719染劑分子結構；(b)N719染劑分子吸收光譜圖…………28
圖2-6 染料透過carboxyl groups與TiO2表面形成ester linkages………28
圖 2-7 Nyquist plots對應等效電路電阻電容……………………………29
圖2-8 等效電路模擬圖…………………………………………………29
圖2-9 簡化等效電路模擬圖……………………………………………29
圖2-10 典型塔弗極化曲線圖…………………………………………30
圖2-11 電子轉移控制與質傳控制之互動關係圖……………………30
圖 2-12  S. Iijima首次發表之多壁奈米碳管HRTEM照片…………31
圖2-13 以三層不同Chirality的石墨層捲區構成之多壁奈米碳管示意
        圖……………………………………………………31
圖2-14 奈米碳管結構向量示意圖……………………………………32
圖2-15 單壁奈米碳管的三種結構示意圖：(a)arm-chair、(b)zigzag與(c)chiral……………………………………………………32
圖2-16懸浮觸媒法裝置示意圖…………………………………………33
圖2-17本實驗室所合成單壁奈米碳管之TEM圖：(a)低倍率；(b)高倍率…………………………………………………………33
圖3-1水平式懸浮觸媒CVD裝置圖…………………………………46
圖3-2產物沉積示意圖…………………………………………………46
圖3-3 (a)絨球狀多壁奈米碳管外觀；(b)多壁奈米碳管之SEM圖…47
圖3-4 DSSC二氧化鈦薄膜之SEM圖………………………………47
圖3-5 染料敏化太陽能電池概要式製作流程圖………………………48
圖3-6 碳極交流阻抗分析測試電池結構圖……………………………49
圖3-7 DSSC對電極量測分析流程圖…………………………………49
圖 4-1片電阻8 □/sq與片電阻15 □/sq導電玻璃之比較：(a)光電轉換效率；(b)全電池照光下EIS分析…………………………………84
圖 4-2 兩不同製程方法鍍鉑金屬於導電玻璃之SEM圖：(a) 濺鍍法
      (sputtering)；(b)熱沉積法(thermal decomposition)……85
圖 4-3 兩不同製程方法鍍鉑金屬於導電玻璃：(a)全電池照光下Nyquist plots；(b)光電轉換效率特性圖…………………………86
圖4-4 相同電池條件下，不同電解液溶劑(ACN or MPN)之比較：(a)光電轉換效率特性圖；(b)全電池照光下Nyquist plots……………87
圖4-5 相同電池條件FTO-TiO2-N719∣0.6 M DMPII or not 0.50 M LiI, 0.05 M I2, 0.5 M TBP in ACN-based electrolyte∣Pt-FTO：(a)光電轉換效率特性圖；(b)全電池照光下Nyquist plots………88
圖4-6 各式碳材所製成的對電極不同倍率SEM表面形貌：(a), (b)nano carbon；(c), (d)MWNTs；(e), (f)LWNTs……………………89
圖4-7 各式對電極之光電轉換特性表現 ……………………………90
圖4-8 再結合損失之飽和再結合電流密度影響填充因子示意圖…90
圖4-9 各式電極於照光下開路電壓條件EIS分析：(a), (b)Nyquist plots；(c), (d)Bode plots………………………………………91
圖4-10 交流阻抗分析對應等效電路圖………………………………91
圖4-11 各式碳極電荷轉移阻抗EIS分析：(a)nano carbon；(b)MWNTs；(c)LWNTs…………………………………………………92
圖4-12 Thermal Pt電極對於電解液([I－]/[ I3－] = 9/1)之循環伏安圖……93圖4-13多次掃描過後，Pt材料在2I3－→3I2 +2e－反應活性 ……………93
圖4-14各式碳極對於電解液([I－]/[ I3－] = 9/1)之循環伏安法圖 ………94
圖4-15 I3－+2e－=3I－反應峰電流值與掃描速率根號關係………94
圖4-16各式對電極對於電解液([I－]/[ I3－] = 9/1)之穩態伏安法圖…95
圖4-17 各式對電極之塔弗曲線圖……………………………………95
圖4-18 膜厚6.05 □m的nano carbon與膜厚為13 □m的MWNTs兩碳
       極穩態伏安圖…………………………………………………96
圖4-19 碳材粉末之TEM分析；(a), (b)多壁奈米碳管(MWNTs)：(c)少壁奈米碳管(LWNTs)：(d), (e)奈米碳粉末(nano carbon)…………97
圖4-20 碳材粉末拉曼光譜(Raman spectrum)；(a) 多壁奈米碳管
(MWNTs)；(b)少壁奈米碳管(LWNTs)；(c)奈米碳粉…………98
圖4-21 Pt/LWNTs電極之SEM表面形貌：(a)50,000X；(b)20,000X；
       (c)側視圖3,500X；(d)側視圖2,000X………………………99
圖4-22 Pt/LWNTs電極並比較thermal Pt、sputtering Pt、LWNTs電極之
     光電轉換特性圖…………………………………………………100
圖4-23 Pt/LWNTs電極並比較thermal Pt、sputtering Pt、LWNTs電極之全電池照光下EIS分析 …………………………………………86
圖4-24 Pt/LWNTs與thermal Pt使用DMPII電解液之光電轉換表現與全
電池照光下EIS分析表現………………………………………101
圖4-25 不同倍率下nano carbon/LWNTs電極之SEM表面形貌：
(a) 50,000X；(b)20,000X………………………………………102
圖4-26 相同條件下，nano carbon/LWNTs電極與LWNTs電極：(a)光電
轉換特性圖；(b)全電池照光下EIS分析 ……………………103
圖4-27 碳材料在染料敏化太陽能電池中對電極要求準則…………104
圖A-1  ED-Pt/LWNTs電極之SEM表面形貌：(a) 50,000X；(b) 20,000X；(c)側視圖3,000X…………………………………………121
圖A-2  不同倍率下ED-Pt鍍於FTO基板之SEM表面形貌：(a) 50,000X；(b) 20,000X ……………………………………………122
圖A-3 (a), (b)EDS分析ED-Pt/LWNTs電極之實驗結果……………123
圖A-4 ED-Pt/LWNTs電極之光電轉換特性表現比較結果……………124









表目錄

表4-1片電阻8 □/sq與片電阻15 □/sq導電玻璃之光電轉換表現與
全電池EIS分析表現……………………………………………77
表4-2 熱沉積Pt與濺鍍Pt之光電轉換表現與全電池照光下EIS分析
     表現…………………………………………………………………77
表4-3 ACN-based電解液與MPN-based電解液之光電轉換表現與照光
     下EIS分析表現……………………………………………………77
表4-4 添加DMPII電解質於ACN-based電解液之光電轉換特性
  表現…………………………………………………………………78
表4-5 添加DMPII電解質於ACN-based電解液之照光下全電池EIS
分析…………………………………………………………………78
表4-6 碳極材料粉末BET、BJH實驗結果………………………………79
表4-7 各式碳極的單位面積厚度之薄膜重量與單位厚度反應面積…79
表4-8 各式碳電極的片電阻(sheet resistance)與電阻率(Resistivity)……80
表4-9 各式碳極光電轉換表現實驗結果………………………………80
表4-10 各式碳極電荷轉移阻抗分析結果………………………………81
表4-11 各式對電極循環伏安法實驗結果………………………………82
表4-12 Pt/LWNTs相較於thermal Pt、sputtering Pt與LWNTs之光電轉
換表現……………………………………………………………82
表4-13 Pt/LWNTs與thermal Pt使用DMPII電解液之光電轉換表現…83
表4-14 nano carbon/LWNTs與LWNTs之光電轉換表現 ………………83
表A-1 ED-Pt/LWNTs電極光電轉換效率之比較………………………120

                                

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