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研究生: 黃仕堯
Huang, Shi-Yao
論文名稱: 缺陷在二維混合有機無機鹵化物鉛鈣鈦礦中的影響
Influence of defects in Two-Dimensional hybrid organic-inorganic halide lead perovskites
指導教授: 劉沂欣
Liu, Yi-Hsin
口試委員: 劉沂欣
Liu, Yi-Hsin
李君婷
Li, Chun-Ting
高琨哲
Kao, Kun-Che
口試日期: 2024/07/03
學位類別: 碩士
Master
系所名稱: 化學系
Department of Chemistry
論文出版年: 2024
畢業學年度: 112
語文別: 中文
論文頁數: 108
中文關鍵詞: 二維有機-無機鈣鈦礦配體輔助再沉澱法聚(甲基丙烯酸甲酯) 鈍化氧氣缺陷
英文關鍵詞: two-dimensional organic-inorganic perovskites, ligand-assisted reprecipitation, PMMA passivation, oxygen, defect
研究方法: 實驗設計法
DOI URL: http://doi.org/10.6345/NTNU202401707
論文種類: 學術論文
相關次數: 點閱:71下載:2
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  • 在本研究中,我們成功利用配體輔助再沉澱法 (ligand-assisted reprecipitation method, LARP 在 室 溫條件下 ((< 合成了二維 層狀 有機無機鈣鈦礦奈米片 。透過引入短碳鏈乙二胺陽離子作為橋接配體,控制了合成溫度和反溶劑比例,從而優化奈米片的生長 。使用穿透式電子顯微鏡與高解析粉末 X光繞射鑑定二維形貌與晶體結構 此鈣鈦礦半導體之層間距小於 1 nm (約 0.8 Å 與先前其他實驗室用以二胺合成之樣品更 具有強烈的量子侷限效應。其中透 螢光光譜發現低溫合成之樣品具有 (390 nm) 和 (500 nm) 兩組 螢光推測低溫樣品具有表現出出色的光學性質 ,並展 現出紫外至可見光範圍( 320 nm)的吸收和發射特性,以及約 3.7 eV的高帶隙,源於量子和介電限制 ,及 為提高材料穩定性,我們採用聚甲基丙烯酸甲酯( PMMA)進行了鈍化,包括共沉澱法和後修飾法。不僅提升了奈米片在氮氣和氧氣環境下的光學性能,而 且通過穿透式電子顯微鏡 、 螢光光譜、疏水性 確認了 PMMA鈍化 奈米片 表面缺陷的 形貌。此外,比較了乾燥箱與手套箱 及大氣下備樣與 氮 氣 環境下備樣 以及不同存放時間 氧氣 對樣品晶格的影響。低溫合成之 樣品 出色的光學性質期待應用於 LED應用而高溫合成之樣品。高溫合成之樣品不發光的特性 未來將聚焦於進一步的光電流研究,探索其在光電應用中的潛力。 最後發現共沉澱法具有鈍化晶體內的缺陷能力同時也能鈍化晶體表面的缺陷,而後修飾法鈍化晶體表現的能力更為出色。

    In this study, we successfully synthesized two-dimensional layered organic-inorganic perovskite nanosheets at room temperature (<100°C) using the ligand-assisted reprecipitation method (LARP). By introducing short-chain ethylenediamine cations as bridging ligands, we controlled the synthesis temperature and antisolvent ratio to optimize the growth of the nanosheets. The two-dimensional morphology and crystal structure were characterized using transmission electron microscopy and high-resolution powder X-ray diffraction. The perovskite semiconductors demonstrated an interlayer spacing of less than 1 nm (approximately 0.8 Å), exhibiting stronger quantum confinement effects compared to samples synthesized with diamines in other laboratories. Photoluminescence spectroscopy revealed two fluorescence groups at 390 nm and 500 nm in samples synthesized at low temperatures, indicating exceptional optical properties with absorption and emission characteristics ranging from UV to visible light (320 nm) and a high bandgap of about 3.7 eV due to quantum and dielectric confinement. To enhance material stability, we utilized polymethyl methacrylate (PMMA) for passivation using both coprecipitation and post-modification methods. This not only improved the optical performance of the nanosheets in nitrogen and oxygen environments but also confirmed the morphology of PMMA-passivated surface defects through transmission electron microscopy, fluorescence spectroscopy, and hydrophobicity tests. Additionally, we compared the effects of oxygen on the lattice of the samples prepared under atmospheric and nitrogen conditions in a dry box and glove box over different storage durations. The outstanding optical properties of the low-temperature synthesized samples hold promise for LED applications, while the non-luminescent characteristics of the high-temperature synthesized samples will focus on further photoelectric current research to explore their potential in photonic applications. Finally, it was found that the coprecipitation method could passivate both internal and surface defects of the crystals, whereas the post-modification method showed superior ability to passivate the crystal defects.

    摘要 i Abstract ii 目錄 iv 第一章 緒論 1 1.1鈣鈦礦半導體之概要 1 1.1.1 光伏效應 2 1.1.2 二維鈣鈦礦和三維鈣鈦礦之比較 2 1.1.3鈣鈦礦相的分類與特性 3 1.2 以化學方法製備鹵素鈣鈦礦半導體 7 1.2.1 熱注射法 (hot injection, HI) 7 1.2.2 配體輔助再沉澱法 (ligand-assisted reprecipitation, LARP) 8 1.3 鈣鈦礦的缺陷與穩定性 9 1.3.1 氧氣對鈣鈦礦之影響 11 1.4 有機高分子在鈣鈦礦中的應用 12 1.5 利用高分子鈍化二維單層雙胺類有機-無機鈣鈦礦奈米片之研究動機 13 第二章 實驗方法 14 2.1 化學藥品 14 2.2 銫前驅物之合成 15 2.3 鉛-乙二胺陽離子前驅物之合成 15 2.4 二維鈣鈦礦奈米片之合成及純化 16 2.4.1 銫-鉛前驅物混合溶液 16 2.4.2 沉澱 16 2.4.3 純化 17 2.5 共沉澱法鈍化奈米片 18 2.6 有機高分子鈍化劑濃度之配置 18 2.7 後修飾法鈍化奈米片 19 2.8 儀器鑑定 20 2.8.1 穿透式電子顯微鏡(Transmission Electron Microscopy, TEM) 20 2.8.2 反射式紫外-可見光吸收光譜儀(Diffuse Reflectance UV-visible Spectrophotometer, DRS) 20 2.8.3 紫外-可見光吸收光譜儀(UV-visible Spectrophotometer, UV-vis) 21 2.8.4 螢光光譜儀(Photoluminescence Spectrophotometer, PL) 21 2.8.5 常溫X光粉末繞射儀(Powder X-ray Diffraction, PXRDs) 22 2.8.6 接觸角測量儀(Contact angle meter) 23 2.8.7 化學分析電子能譜儀(Electron Spectroscopy for Chemical Analysis, ESCA) 23 2.9名稱統整縮寫 24 第三章 結果與討論 25 3.1 合成溫度及反溶劑對結晶度之影響 25 3.1.1 合成溫度及反溶劑對晶體生長之影響 26 3.1.2 反溶劑(hexane, toluene, methanol)對電子結構之影響 39 3.2 氧氣對二維鈣鈦礦奈米片之影響 45 3.2.1 氧氣對晶格生長之影響 45 3.2.2 晶體表面的缺陷 62 3.3 以有機高分子鈍化二維鈣鈦礦奈米片 64 3.3.1 共沉澱法鈍化奈米片 64 3.3.2 後修飾法鈍化奈米片 76 第四章 結論 94 參考資料 96 附錄 105 S1.1 二維有機無機鈣鈦礦螢光半生期 105

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