臺灣博碩士論文加值系統

本研究重點為無乳化聚合法(Emulsifier-free Emulsion Polymerization)製備聚苯乙烯(Polystrene; PS)微球後，利用硬模板法(Hard-Templating Method)製備二氧化鈦中空微球，並以電泳自組裝(Electrophoretic Deposition Self-Assembly; EPSA)方法，製作PS模板；再利用溶膠凝膠法(Sol-gel)製備二氧化鈦反蛋白石(Titania Inverse Opal; TIO)結構。最後將TiO2中空球與反蛋白石結構應用於染料敏化太陽能電池(Dye Sensitized Solar Cell; DSSC)。研究結果得知，吾人以無乳化聚合法搭配陽離子型起始劑AIBA (2,2,Azobis(2-Methylpropion Amidine) Dihydrochloride)合成表面帶正電荷之PS微球作為模板，利用硬模板法合成TiO2/PS核殼微球，經由450oC煆燒移除PS模板後，可獲得具有銳鈦礦晶相之TiO2中空微球。異丙醇鈦濃度為0.1 M所製備之TiO2中空微球，有著最高比表面積為89.35 m2/g，其染料敏化太陽能電池之光電效率也達到1.5%，勝於商用P25粉體。吾人亦利用EPSA技術有效率地獲得高完整性之PS光子晶體模板，藉由Sol-gel法將TiO2膠體填入PS模板孔隙之中，再經由高溫煆燒移除模板能獲得具有銳鈦礦晶相且無雜質之TIO結構，其光電轉換效率為0.1%。

The main aims of this study are to use the emulsifier-free polymerization to produce polystyrene (PS) microspheres, which were used in the hard-templating method to form titania hollow microsphere. Furthermore, we prepared PS photonic crystal template via electrophoresis self-assembly (EPSA) method, sussequently such photonic crystal templates were used to form a titania inverse opal (TIO) structure via sol-gel method. Both independent titania hollow microspheres and TIO structure serve as the working electrodes in dye-sensitized solar cells (DSSCs) for studying the change of DSSC efficiency. The surfaces of PS microspheres derived from emulsifier-free polymerization with cationic initiator of 2,2,azobis(2-methylpropion a midine) dihydrochloride (AIBA) are associated with positive charges. In hard-templating method, titanium(IV) isopropoxide (TTIP) was used as precursor to produce TiO2/PS core shell microspheres to begin with PS microsphere templates. Finally, TiO2 hollow microspheres with anatase phase were obtained after calcination at 450oC to remove PS templates. Those TiO2 hollow microspheres derived from TTIP of 0.1 M concentration have rather higher specific surface area of 89.35 m2/g. The efficiency of DSSC with electrode of TiO2 hollow microsphere was 1.5 %, which was higher than that of electrode made of commercial titania P25 powders. The 3-D photonic crystal templates with opal structure were easily frabricated by EPSA technique. After voids of PS template were filled up with titania sol, TIO structures of anatase crystalline phase without any imputrities were successfully synthecized by removing the PS microspheres through pyrolysis and calcination. The results indicate that TIO has poor continuity, which led to rather low photoelectric conversion efficiency for DSSCs at 0.1% level.

摘 要 I
英文摘要 II
目錄 III
圖目錄 VII
表目錄 XII
第一章 緒 論 1
1.1太陽能電池發展與應用 1
1.2太陽能電池之總類 4
1.3中空結構之簡介與應用 10
1.4光子晶體簡介 11
1.5反蛋白石光子晶體 14
1.6電泳自組裝技術發展介紹 16
1.7研究目的與重點 18
第二章 理論基礎 22
2.1染料敏化太陽能電池 22
2.1.1染料敏化太陽能電池概述 22
2.1.2染料敏化太陽能電池基本構造與工作原理 23
2.1.3透明導電玻璃 25
2.1.4二氧化鈦(TiO2)工作電極 26
2.1.5染料(Dyes) 31
2.1.6電解液(Electrolytes) 34
2.1.7白金對電極(Pt Counter Electrode) 35
2.1.8染料敏化太陽能電池元件數據量測 36
2.2高分子微球的製作 39
2.3二氧化鈦中空球製程 40
2.4光子晶體模板與反蛋白石光子晶體製程 42
第三章 實驗步驟與方法 47
3.1無乳化聚合法製備聚苯乙烯微球 47
3.2硬模板法合成二氧化鈦中空微球 50
3.3硬模板法製備TiO2中空微球相關反應參數 51
3.3.1煆燒溫度對TiO2中空微球之影響 51
3.3.2煆燒持溫時間對TiO2中空微球之探討 51
3.3.3異丙醇鈦濃度對TiO2中空微球之研究 51
3.3.4反應時間對TiO2中空微球之相依性 52
3.4電泳自組裝PS微球形成光子晶體模板 52
3.5溶膠凝膠法製備二氧化鈦反蛋白石結構 54
3.6 Sol-Gel法製備TIO結構相關反應參數 55
3.6.1浸泡時間對TIO結構之影響 55
3.6.2重複浸泡回數對TIO結構之影響 56
3.6.3乾燥時間對TIO結構之影響 56
3.6.4異丙醇鈦濃度對TIO結構之影響 56
3.7染料敏化太陽能電池全電池封裝 57
3.7.1基板清洗 57
3.7.2二氧化鈦工作電極製備 58
3.7.3浸泡染料 60
3.7.4對電極製備 60
3.7.5 DSSC全電池封裝 60
3.8 分析儀器 61
3.8.1 冷場發射掃描式電子顯微鏡 61
3.8.2 多功能薄膜X光繞射儀 63
3.8.3 穿透式電子顯微鏡 64
3.8.4 示差掃描量熱-熱重分析聯用儀 64
3.8.5 比表面積分析儀 66
3.8.6 Zeta介面電位分析儀 67
3.8.7 太陽光模擬器 69
第四章 結果與討論 70
4.1無乳化聚合法製備聚苯乙烯微球 70
4.2硬模板法合成二氧化鈦中空微球 72
4.2.1煆燒溫度對TiO2中空微球之影響 72
4.2.2煆燒持溫時間對TiO2中空微球之探討 76
4.2.3異丙醇鈦濃度對TiO2中空微球之研究 78
4.2.4反應時間對TiO2中空微球之相依性 80
4.2.5煆燒溫度對TiO2中空微球之晶相分析 82
4.2.6 TiO2中空微球之比表面積分析 83
4.2.7 TiO2中空微球應用於染料敏化太陽能電池之效率分析 87
4.3溶膠凝膠法製備二氧化鈦反蛋白石結構 94
4.3.1浸泡時間對TIO結構之影響 94
4.3.2浸泡回數對TIO結構之影響 96
4.3.3乾燥時間對TIO結構之影響 97
4.3.4異丙醇鈦濃度對TIO結構之影響 97
4.3.5 二氧化鈦反蛋白石結構之晶相分析 101
4.3.6 二氧化鈦反蛋白石結構之元素分析 101
4.3.7 TiO2反蛋白石結構應用於DSSC之效率分析 104
4.6未來研究方向 105
第五章 結 論 109
參考文獻 111

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