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研究生： 郭衣紜
Yi-Yun Kuo
論文名稱： 鈣鈦礦發光二極體之研究
The Study of Perovskite Light Emitting Diodes
指導教授： 陳良益
Liang-Yih Chen
口試委員: 陳貞夙
Jen-Sue Chen
吳季珍
Jih-Jen Wu
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： 2022
畢業學年度： 110
語文別： 中文
論文頁數： 199
中文關鍵詞： 無機載子傳輸層 、發光二極體 、晶粒奈米化
外文關鍵詞： inorganic carrier transport layer, light-emitting diode, nanocrystal pinning
相關次數： 點閱：821  下載：2 
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    • 本研究先將電洞注入層替換成氧化鎳對進行其表面形貌、光學性質及發光二極體光電特性分析。由以上分析結果證實鈣鈦礦薄膜需要進一步的優化。因此在後續進行兩種不同的方法進行鈣鈦礦的優化製程，第一種是透過旋塗過程中滴入反溶劑拿到晶粒奈米化，並搭配聚甲基丙烯酸甲酯進行鈍化處理。另一種則是透過添加聚乙烯吡咯烷酮進入鈣鈦礦溶液達到原位生成奈米化晶粒。最終以聚乙烯吡咯烷酮添加5 毫克每毫升為最佳條件，對其表面覆蓋率、螢光效率、激子輻射再結合率都有提升。所製備的鈣鈦礦薄膜發光二極體之光電效能為：啟動電壓 2.90 V，最大輝度 2035 cd/m2、最大電流效率 21.72 cd/A以及外部量子效率 6.83 %。並經由 20組發光二極體的效能分析，在本研究中可獲得的鈣鈦礦薄膜發光二極體最高外部量子效率可達 8.60 %。接續將電子傳輸層替換成無機的氧化鋅，但受限於氧化鋅對鈣鈦礦結構的劣化。在應用製發光二極體時，啟動電壓沒有變動，輝度降至1102 cd/m2上，且在外部量子效率降低至0.14 %。

    In recent years, the mainstream materials of carrier transport layers for perovskite light-emitting diodes still occupied by various organic small molecules and conductive polymers in the field. However, inorganic carrier transport layers seem to be the better choice, as many research groups have proposed that they are more stable in harsh environments. In this study, the hole injection layer was replaced by nickel oxide and analyzed the surface morphology, optical properties and photoelectric properties of light-emitting diodes. From the above analysis results, it is confirmed that the perovskite film needs to further optimizate. Therefore, two different methods are used to optimize the perovskite. The first one is to drop the anti-solvent during the spin coating process to reach nanocrystal pinning effect, and passivate it with polymethyl methacrylate. The other is to produce nanocrystalized perovskite in situ by adding polyvinylpyrrolidone into the perovskite solution. Finally, adding 5 mg/ml of polyvinylpyrrolidone was the optimal condition, and its surface coverage, fluorescence efficiency, and exciton radiation recombination rate were improved. The performances of perovskite TF-LEDs were: turn-on voltage of 2.90 V, maximum luminance of 2035 cd/m2, maximum current efficiency (CE) of 21.72 cd/A and external quantum efficiency(EQE) of 6.83%. The highest external quantum efficiency in this study could achieve 8.60%, which was obtained by analyzing 20 sets of perovskite TF-LEDs. The electron transport layer was subsequently replaced with inorganic zinc oxide, but it was limited by the deterioration of the perovskite structure by zinc oxide deposition. The performances of perovskite TF-LEDs were: turn-on voltage of 2.90 V, maximum luminance of 1102 cd/m2, and EQE of 0.14%.

    摘要 I Abstract II 致謝 IV 目錄 VI 圖目錄 XIV 表目錄 XXVIII 第一章、緒論 1 1-1前言 1 1-2研究動機與目的 2 第二章、理論基礎與回顧 3 2-1 半導體與奈米材料 3 2-1-1 半導體概念與能帶圖 3 2-1-2 量子井結構 6 2-2 鈣鈦礦材料 8 2-2-1 鈣鈦礦結構 8 2-2-2 鈣鈦礦材料發展 11 2-3 鈣鈦礦發光二極體 13 2-3-1 發光二極體與各層結構介紹 13 2-3-2 發光二極體的工作原理 16 2-3-3 載子傳輸層材料的選擇 17 2-3-4 發光二極體效能指標介紹 20 2-3-4-1 啟動電壓(turn-on voltage，VTO) 20 2-3-4-2 LED發光程度的單位 20 2-3-4-3 電流效率(current efficiency，CE) 24 2-3-4-4 外部量子效率(external quantum efficiency，EQE) 24 2-3-4-5 電子主導與電洞主導元件之分析與計算 27 2-4 鈣鈦礦發光二極體的優化近期研究及其優化製程 31 2-4-1 降低鈣鈦礦晶體尺寸 31 2-4-2 缺陷鈍化與介面工程 34 2-4-3 鈣鈦礦與高分子混合 39 2-4-4 傳輸層調整與替換 42 2-4-5 近期鈣鈦礦發光二極體整理 48 第三章、實驗設計 51 3-1 實驗流程圖 51 3-2 實驗藥品 52 3-3 實驗儀器與分析原理 57 3-3-1 超音波震盪器 (Ultrasonic cleaner) 57 3-3-2 攪拌式加熱板 (Hot plate) 57 3-3-3 管式高溫爐 (Tube furnace) 57 3-3-4 微量天平 (Electronic balance) 58 3-3-5 外光燈 (UV lamp) 58 3-3-6 旋轉塗佈機 (Spin coater) 58 3-3-7 手套箱 (Glove box) 59 3-3-8 金屬蒸發源系統 (Metal evaporation source system) 60 3-3-9 紫外光-可見光光譜儀(UV/visible spectrophotometer) 61 3-3-10 X光繞射分析儀(X-ray diffraction，XRD) 62 3-3-11 場發射穿透式電子顯微鏡 (Field-emission gun transmission electron microscope，FETEM) 64 3-3-12 時間解析光致發光測量系統(Time-resolved photoluminescence，TRPL) 66 3-3-13 紫外光電子能譜儀（Ultraviolet Photoelectron Spectroscopy，UPS） 68 3-3-14 高解析度場發射型掃描式電子顯微鏡 (High Resolution Field-emission Scanning Electron Microscope，HRFE-SEM) 70 3-3-15 電致發光量測系統(Electroluminescence，EL) 71 3-4 實驗步驟 72 3-4-1 氧化鎳前趨溶液配置 72 3-4-2 氧化鋅奈米顆粒溶液置備 73 3-4-3 Pristine鈣鈦礦溶液配置 74 3-4-4 PVP鈣鈦礦溶液配置 74 3-4-5 發光二極體的製備 75 3-4-5-1.定義工作面積與清洗ITO導電玻璃 75 3-4-5-2.旋轉塗佈電洞注入層/電洞傳輸層 76 3-4-5-3.旋轉塗佈鈣鈦礦層 77 3-4-5-4. 熱蒸鍍電子傳輸層、電子注入層與陰極與封裝(與3-4-4-5節擇一) 77 3-4-5-5. 旋轉塗佈電子傳輸層、熱蒸鍍電子注入層與陰極與封裝(與3-4-4-4節擇一) 78 3-4-6 電洞主導元件的製備 79 3-4-5-1.定義工作面積與清洗ITO導電玻璃 79 3-4-5-2.旋轉塗佈電洞注入層/電洞傳輸層 80 3-4-5-3.旋轉塗佈鈣鈦礦層 81 3-4-5-4.熱蒸鍍電洞傳輸層與金電極與封裝 82 3-4-7 電子主導元件的製備 82 3-4-7-1.定義工作面積與清洗ITO導電玻璃 82 3-4-7-2.熱蒸鍍電子傳輸層 83 3-4-7-3.旋轉塗佈鈣鈦礦層 84 3-4-7-4. 熱蒸鍍電子傳輸層、電子注入層與陰極與封裝 84 第四章、結果與討論 86 4-1 探討以NiO作為電洞注入層對鈣鈦礦發光元件效能之影響 86 4-1-1 無機電洞注入層NiO基本性質分析 86 4-1-2 以NiO為電洞注入層製作鈣鈦礦綠光二極體效能分析 92 4-2 鈣鈦礦綠光二極體製程優化探討 104 4-2-1 探討以不同溶劑進行nanocrystal pinning處理對鈣鈦礦綠光二極體效能之影響 104 4-2-2 探討添加PMMA進行nanocrystal pinning處理對鈣鈦礦綠光二極體效能之影響 113 4-2-3 探討添加PVP對鈣鈦礦綠光二極體效能之影響 128 4-3 以ZnO電子傳輸層應用於鈣鈦礦綠光二極體的效能探討 142 4-3-1 ZnO電子傳輸層基本性質分析 142 4-3-2 以全無機載子傳輸層製作鈣鈦礦綠光二極體效能分析 145 第五章、結論 151 第六章、參考文獻 153

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