臺灣博碩士論文加值系統

在本文中，我們受到熱注射法的啟發，在熱注射法的基礎上改良出了一種強大的熱添加法（Hot addition method）。其可解決過去高溫下有機陽離子易分解而不適用於合成有機-無機鈣鈦礦奈米晶體的困難，使此方法合成出高結晶性和穩定度的有機 - 無機鈣鈦礦奈米晶體，且具有很高的光致發光量子產率和可調光學。
利用熱添加法成功合成CsFAPbBr3、MAPbBr3，證明熱添加法適用於多種有機陽離子。此外藉由熱注射法製備CsPbBr3、熱添加法與熱注射法並用合成CsFAPbBr3和多種不同合成法合成MAPbBr3，探討不同陽離子及不同合成製程對鈣鈦礦奈米晶體的光學性質影響。之後選擇固相-氣相催化反應條件進行藍光下的光催化反應，並嘗試以光學性質的差異解釋不同鈣鈦礦奈米晶體光催化效率的表現，由於MAPbBr3放光生命週期較長，容易傳遞激發電子進行二氧化碳還原反應，故MAPbBr3相較其他陽離子含鉛鈣鈦礦有較優異表現，其中又以加入微量水參與反應合成出地MAPbBr3有最佳的催化效能和穩定性。

將鈣鈦礦奈米晶體在光伏轉換應用的方面，亦使用熱添加法製備MAPbCl3和摻雜Mn2+的MAPbCl3（Mn：MAPbCl3）鈣鈦礦納米晶體，用於發展發光型太陽能集光器（LSC）的應用。其中 Mn：MAPbCl3 鈣鈦礦奈米晶體顯示出顯著的斯托克斯位移高達200nm。藉由此特性製備以MAPbCl3和Mn：MAPbCl3為發光介質的太陽能集光器元件，元件具有一定透光度同時顯示出1.2％和3.3％的優異導光率，且因為Mn摻雜造成的高斯托克移位（200nm）抑制了發光介質的再吸收，使太陽能集光器放大後導光率仍不受影響。

In this thesis, we have devolped a robust hot-addition method (HAM) inspired by the hot injection method. HAM can solve the problem that the organic cation is easily decomposed at high temperature which cause difficulty for synthesizing the organic-inorganic hybrid perovskite nanocrystals. The HAM can synthesize highly crystalline and stable organic-inorganic perovskite nanocrystal with great photoluminescent quantum yield and tunable optical properties.
The MAPbBr3 and CsFAPbBr3 were successfully synthesized by the hot addition method, which proved that the HAM is applicable to various organic cations. The effects of different A cations and different synthetic processes on the optical properties of perovskite nanocrystals were investigated by following perovskite nanocrystals. CsPbBr3 was prepared by hot injection method. CsFAPbBr3 was generated by combining hot injection method and HAM. MAPbBr3 was synthesized by three different synthesis methods. The photocatalysis reactions chosen under solid-gas phase reaction conditions were carried out under blue LED light. Then, the differences in optical properties were used to explain the photocatalysis performance of different perovskite nanocrystals. Since MAPbBr3 photoluminescence lifetime is longer which let excited electrons can easily transmit for reduction reaction, MAPbBr3 has better performance than other component lead halide perovskites. Among the three types MAPbBr3, the MAPbBr3 synthesized by the participation of trace water in the reaction show superior catalytic activity and stability.
In addition, MAPbCl3 and Mn-doped MAPbCl3 (Mn: MAPbCl3) were prepared by HAM for the development of luminescent solar concentrator (LSC) applications. The Mn:MAPbCl3 perovskite nanocrystals show a remarkable Stokes shift up to 200 nm. Based on this property, solar concentrators had fabricated with MAPbCl3 and Mn:MAPbCl3 as the luminescent medium. The device still retain a certain transmittance while exhibiting high optical efficiencies of 1.2% and 3.3%, respectively. However, efficiency of LSC remained unaffected after enlargment of LSC device because high stoke shift (200nm) achieved by Mn doping supresses re-absorption of emitted photon.

摘要 i
Abstract iii
誌謝 v
目錄 vi
圖目錄 x
表目錄 xv
第 一 章 緒論 - 1 -
第 二 章 文獻回顧 - 3 -
2-1 鈣鈦礦材料性質(Perovskite)1 - 3 -
2-2 鈣鈦礦奈米晶的發展 - 6 -
2-3 鈣鈦礦奈米晶膠體合成法 - 11 -
2-3-1由上而下法(Top down Method) - 12 -
2-3-2配體輔助再沉澱法（ligand-assisted reprecipitation, LARP） - 12 -
2-3-3熱注射法(Hot Injection method, HI) - 15 -
2-4 鈣鈦礦光催化反應 - 22 -
2-4-1光催化還原二氧化碳反應機制 - 22 -
2-4-2鈣鈦礦光催化反應的發展 - 24 -
2-5 太陽能集光器簡介 - 27 -
2-5-1太陽能集光器發展 - 27 -
2-5-2 導光式太陽能集光器工作原理 - 34 -
2-5-3 導光式太陽能集光器基本特性分析 - 36 -
2-6 研究動機 - 37 -
第 三 章 實驗步驟與方法 - 39 -
3-1 實驗藥品及儀器 - 40 -
3-1-1實驗材料 - 40 -
3-1-2實驗儀器 - 43 -
3-2實驗步驟 - 45 -
3-2-1合成鈣鈦礦納米晶 - 46 -
3-2-2光催化還原實驗操作 - 50 -
3-2-3製備發光型太陽能聚光器元件 - 52 -
3-3 奈米晶體定性檢測 - 54 -
3-3-1分光光譜儀(UV/ Vis / NIR Spectrophotometer, UV/ Vis) - 54 -
3-3-2螢光放光光譜儀 (Photoluminescence spectroscopy, PL) - 54 -
3-3-3感應耦合電漿原子發射光譜儀(Inductively Coupled Plasma Optical Emission Spectrometry, ICP-OES) - 55 -
3-3-4穿透式電子顯微鏡(TEM) - 55 -
3-3-5 X射線繞射分析(XRD) - 56 -
3-3-6時間相關單光子計數光譜(Time-correlated single photon counting , TCSPC) - 56 -
3-4 光催化反應產物分析 - 57 -
3-4-1氣相層析火焰離子化偵檢器(GC-FID) - 57 -
3-4-2高解析氣相層析質譜儀(HRGC-Mass) - 57 -
3-5 太陽能集光器元件量測 - 59 -
3-5-1太陽能集光器量測前處理 - 59 -
3-5-2光電轉換效率的量測 - 59 -
3-5-3 入射單色光子-電子轉化效率量測(IPCE) - 61 -
3-5-4分光光譜儀(UV/ Vis / NIR Spectrophotometer, UV/ Vis) - 61 -
第 四 章 APbBr3光催化反應之結果與討論 - 62 -
4-1 APbBr3吸收與螢光放光光譜 - 64 -
4-2鈣鈦礦奈米晶 XRD 薄膜繞射 - 66 -
4-3 APbBr3時間相關單光子計數光譜 - 68 -
4-4 選擇光催化反應之反應條件 - 71 -
4-5 光觸媒APbBr3之光催化產量比較 - 73 -
4-6 結論 - 76 -
第 五 章 MAPbCl3應用於太陽能集光器之結果與討論 - 78 -
5-1 比較不同合成方法製備鈣鈦礦奈米晶體UV-Vis吸收光譜穩定性差異 - 79 -
5-2熱添加法製備不同比例Mn:MAPbCl3光學性質比較 - 81 -
5-3 Mn2+反應性與對鈣鈦礦奈米晶體結晶的影響 - 83 -
5-4穿透式電子顯微鏡統計鈣鈦礦奈米晶尺寸 - 85 -
5-5發光型太陽能聚光器光電轉換效率與導光效率計算 - 87 -
5-6發光型太陽能聚光器導光效率與導光聚合物穿透度比較 - 91 -
5-7大面積發光型太陽能聚光器光電轉換效率 - 93 -
5-8 發光型太陽能聚光器元件穩定度 - 94 -
5-10 結論 - 95 -
參考文獻 - 97 -
附錄 - 104 -
附錄一 甲烷檢量線 - 104 -
附錄二 一氧化碳檢量線 - 104 -
附錄三 氣相層析質譜儀鑑驗報告 - 105 -
附錄四 工研院檢驗報告 - 110 -

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