近年來鹵化鈣鈦礦之研究發表於光電領域之表現突飛猛進，使該材料得到了越來越多的關注。其對可見光優異的吸收能力、光致放光量子產率、能隙可調性以及近年來被大量研究的單光子放光特性，使其能夠應用之領域不僅止於顯示以及照明之應用。但其水氧穩定性不佳以及會將鉛釋放到環境中之可能性仍是其投入實際商業化之一大阻礙。
本篇論文主要針對甲脒基含鉛鈣鈦礦量子點以及薄膜之製程進行參數優化與改質，試圖使其性質更加貼近實際應用端之需求並改善因其天生離子性所導致的不穩定性。
於本論文第一章中簡單介紹了鹵化鈣鈦礦之結構、特性以及其近年之發展並且對後須實驗中會進行量測的光學性質說明了其原理以及代表的物理意義。
第二章簡單介紹了現今常用於鈣鈦礦量子點合成的製程並說明了前驅物、配體等選擇的根據以及實驗設計之邏輯。並且介紹了本實驗室之光致放光頻譜、量子產率、吸收頻譜以及時間解析光致放光量測之實驗架設。對初步嘗試製程合成量子點之光學性質提出了可能之解釋並提出後續製程改良之方向。
於第三章中對鈣鈦礦量子點進行了製程參數之優化。首先對熱注入法，透過前驅物比例調整成功將其光致放光波長，將初步嘗試之青綠色調整至更適合顯示器應用之CIE座標上Rec2020.綠色端點，並且針對該前驅物比例進一步提高製程持溫時間在使其更進一步接近Rec2020.的同時將其光致放光量子產率提升至90%，並且也成功合成出量子產率100%之鈣鈦礦量子點。針對配體輔助再析出法也嘗試透過配體的調整將其光致放光量子產率提升至約80%。並於本章結最後介紹了單光子源特性以及量測架設後對合成之量子點進行單光子源特性量測得到其具備極高的單光子純度g(2)(0)~0.04。
第四章中嘗試了準二維鈣鈦礦量子點之合成並發現其性質因量子點分散特性導致其與預期不相符，因此轉為進行準二維鈣鈦礦薄膜之合成之研究。於合成開始前引入了本研究團隊與清大周鶴修教室實驗室合作設計之分子4PhMA，透過電致發光元件工作原理以及準二維鈣鈦礦特性闡述其分子設計邏輯，並在簡單介紹製程後，對4PhMA合成準二維鈣鈦礦薄膜進行大量的製程參數優化找出最佳化之前驅物與退火條件。並且展示了可供參考之薄膜厚度調整參數以及透過鹵素混摻調整能隙，之後更是測試A site陽離子之混摻與置換與結果。對準二維鈣鈦礦薄膜進行了UPS量測其最高佔據軌域能階並透過其能隙推測最低未佔據軌域能階。透過掃瞄式及穿透式電子顯微鏡觀察薄膜之表面形貌以及內部微結構並透過EDX對其進行元素分析。以瞬態吸收量測作為準二維鈣鈦礦薄膜中能量轉移的直接證據。GIWAXS量測結果則證明了4PhMA促進高效率之亞穩態α-phase之形成以及保護效果。ICP-MS量測則更為直接的表現了4PhMA準二維鈣鈦礦薄膜之水穩定性。
第五章中提出準二維鈣鈦礦薄膜水穩定性使其具備用於光催化產氫之可能性。根據第四章結尾之量測結果所得到的能帶結構選擇了適合作為共催化劑之PCBM，並且測試了準二維鈣鈦礦薄膜於犧牲試劑TEOA水溶液下之穩定性。透過製程參數調整成功製備了接近1:1體積比之準二維鈣鈦礦與PCBM異質接面並於之後進行光催化產氫實驗，並根據其結果提出結果不理想之可能性。
於第六章總結了本研究的兩大部分並且提出未來之研究方向。

Lead halide perovskites have been intensively studied in recent years due to its’ excellent optical properties, including high absorption cross section, photoluminescence quantum yield, tunable band gap and its single photon properties. Lots of research have been done on lead halide perovskite, which makes it develop at breakneck speed. However, the instability toward the ambient environment inherent from its ionic characteristics greatly hinder the commercialization of halide perovskite.
This thesis can be categorized in two main part. One is the fabrication and optimization of formamidinium lead bromide perovskite quantum dots and the other one is the fabrication and optimization of quasi-2D formamidinium lead iodide perovskite.
In the first chapter, the structure、properties and recent development of lead halide perovskite quantum dots and quasi-2D perovskite were briefly reviewed. Then working principle behind several optical properties including time-resolved photoluminescence, photoluminescence spectrum, absorbance, transient absorption, and CIE 1931 color space along with their physical meaning were introduced.
In the second chapter, two most commonly applied chemical synthesis method of perovskite quantum dots, hot-injection and ligand-assist reprecipitation were reviewed. Then spray synthesis was applied on these two synthesis to improve the quality of quantum dots. After introducing measurement setup, the PL spectrum, PLQY, time-resolved PL and absorbance for the synthesized quantum dots were shown acting as guideline for modification of synthesis parameters discussed in next chapter.
In third chapter, synthesis was optimized and effects of the experimental parameters on the properties perovskite quantum dots were studied. For hot-injection synthesis, by tuning the ratio between perovskite precursor the emission wavelength of quantum dots was red-shifted from ultramarine to the green color requirement for Rec2020. which was designed to expand color gamut of devices based on human eye response. And the optimization of reaction temperature further increase PLQY of the quantum dots that suitable for green light display up to 90%. The stability of perovskite quantum dots was also tested and the results show that the perovskite quantum dots can survive in air for almost 100 days without significant decay of PLQY and agglomeration. For ligand-assist reprecipitation the ligand OcA was replaced by OAm and the amount of OAm was modified. After optimization, the PLQY of quantum dots synthesized by LARP process was increased from 29% to 76%. Single photon properties were studied after optimization of chemical synthesis to see whether it can act as a single photon emitter. In this chapter perovskite quantum dots with near unity PLQY and ultra-high single photon purity g(2)(0)~0.04 were synthesized.
In fourth chapter, quasi-2D perovskite quantum dots was synthesized and shown to be inefficient. The result was attributed to the average distance between perovskite quantum dots which is too far for Dexter and Förster energy transfer. As a result fabricating quasi-2D perovskite thin film might be better than quantum dots. So a new type of large organic halide 4PhMA act as spacer in quasi-2D perovskite was designed via collaboration between our research group and Prof. Ho Hsiu Chou’s research group and synthesized by Prof. Chou’s lab. The design rationale of 4PhMA was explained by working principle of OLED and quasi-2D perovskite. Then quasi-2D lead formamidinium iodide perovskite thin films were fabricated by 4PhMA. After optimization of precursor solution and annealing condition a perovskite thin film with PL spectrum in NIR, PLQY up to 85% was fabricated which shows unprecedented stability toward oxygen and water. Bandgap of quasi-2D perovskite was tuned through halide mixing with its stability preserved at the same time. After optimization, HOMO and LUMO level were measured and calculated via UPS measurement. And its morphology, micro structure and composition were explored by SEM, TEM and EDX. GIWAXS measurement shows that 4PhMA can help to stabilizeα-phase in lead iodide perovskite better than OcA and PEA. After that, the energy transfer mechanism described in chapter 1 was proofed through transient absorption measurement. In the end of this chapter superior stability was demonstrated through ICP-MS measurement.
In fifth chapter, an experiment about photocatalytic hydrogen evolution was designed based on its water stability. PCBM was chosen to be cocatalyst to form a type II bulk heterojunction which was proofed via PL quenching of quasi-2D perovskite after mixing with PCBM. TEOA was chosen to be sacrificial reagent and its solution was used to test the stability of quasi-2D perovskite thin film. The 4PhMA quasi-2D perovskite thin film was found stable enough to survive in TEOA solution for hours. However, the result shown a very low hydrogen generation rate arise from the unknown mechanism of cosolvent on quasi-2D perovskites which require more detailed measurement to verify.
And in the final chapter all the experimental results above were summarized to provide some direction for future research.

摘要..........................................................I
Abstract ....................................................III
致謝 ........................................................VI
目錄 ........................................................VIII
圖目錄 ......................................................XI
表目錄 ......................................................XVI
第1 章 緒論 ..................................................1
1-1 前言 ....................................................1
1-2 鹵化鈣鈦礦 ...............................................2
1-3 鹵化鈣鈦礦近年之發展 ......................................4
1-4 鹵化鈣鈦礦量子點 ..........................................5
1-5 準二維鈣鈦礦 ..............................................6
1-6 基本光物理特性介紹 ........................................10
1-6-1 光致放光(photoluminescence) ...........................10
1-6-2 光致放光量子產率(photoluminescence quantum yield) .... 11
1-6-3 時間解析光致放光(time-resolved PL).....................11
1-6-4 吸收光譜(absorption) .................................12
1-6-5 光致放光激發頻譜(photoluminescence excitation spectrum).12
1-6-6 瞬態吸收(transient absorption) ........................ 13
1-6-7 CIE 1931 色彩空間 ......................................13
第2 章 有機鹵化鈣鈦礦量子點之合成 ................................16
2-1 鹵化鈣鈦礦量子點製程介紹 ...................................16
2-2 合成FAPbBr3 鈣鈦礦量子點實驗設計 ...........................17
2-2-1 以配體輔助再析出法合成FAPbBr3 鈣鈦礦量子點 ...............18
2-2-2 以熱注入法合成FAPbBr3 鈣鈦礦量子點 ......................19
2-3 光學性質量測簡介 .........................................21
2-3-1 光致放光頻譜量測 .......................................21
2-3-2 光致放光量子產率量測 ...................................21
2-3-3 時間解析光致放光量測 ...................................23
2-3-4 吸收光譜量測 ..........................................24
2-4 鈣鈦礦量子點量測結果 .....................................25
2-5 結論 ...................................................28
第3 章 鈣鈦礦量子點製程優化 ..................................30
3-1 前言 ...................................................30
3-2 熱注入法製程優化 ........................................31
3-2-1 前驅物比例調整 ........................................31
3-2-2 加熱條件調整 ..........................................35
3-2-3 穩定度測試 ............................................39
3-3 配體輔助再析出法製程優化 .................................41
3-3 單光子源介紹與量測 .......................................44
3-3-1 單光子源簡介 ..........................................44
3-3-2 單光子特性之量測 .......................................46
3-3-3 單光子源量測樣品製備 ...................................48
3-3-4 單光子特性量測結果 ...................................48
3-4 小結 ..................................................51
第4 章 準二維鈣鈦礦 ....................................... 53
4-1 前言 .................................................53
4-2 PEA 準二維鈣鈦礦量子點 ................................54
4-2-1 PEA 準二維鈣鈦礦合成 ................................54
4-2-2 合成結果與量測 ......................................55
4-3 有機分子4PhMA 分子設計 ................................59
4-3-1 電致發光元件OLED 工作原理簡介 ........................59
4-3-2 準二維鈣鈦礦之大型有機陽離子 .........................62
4-3-3 有機陽離子分子設計 ..................................64
4-4 準二維鈣鈦礦薄膜製備與量測 .............................65
4-4-1 準二維鈣鈦礦薄膜製程 .................................65
4-4-2 準二維鈣鈦礦薄膜製程參數與量測結果 ....................66
4-4-3 最佳化樣品與穩定性測試 ...............................68
4-4-4 薄膜厚度調整.........................................71
4-4-5 鹵素混摻 ............................................71
4-4-6 A-site 陽離子混摻與置換 ..............................73
4-5 準二維鈣鈦礦性質量測 ...................................76
4-5-1 紫外光電子能譜(UPS) ..................................76
4-5-2 穿透式及掃瞄式電子顯微鏡(SEM&TEM) .....................77
4-5-3 EDX 元素分析 .........................................79
4-5-4 瞬態吸收量測介紹 ......................................80
4-5-5 瞬態吸收量測結果 .....................................83
4-5-6 掠角入射X 光廣角散射(GIWAXS) .........................87
4-5-7 感應耦合電漿質譜(ICP-MS) .............................89
4-6 小結 ..................................................91
第5 章 鈣鈦礦薄膜光催化產氫 .................................94
5-1 前言 ..................................................94
5-2 光催化產氫原理介紹 .....................................94
5-3 準二維鈣鈦礦於溶液中之穩定度測試 ........................96
5-4 混摻PCBM 異質介面 ......................................98
5-5 光催化產氫量測結果與討論 ................................101
5-6 小結 ..................................................105
第6 章 總結與未來展望 .......................................107
參考文獻 ...................................................110

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