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研究生: 傅宇謙
Fu, Yu-Cian
論文名稱: 以化學氣相沉積合成生長錳摻雜鈣鈦礦奈米粒子及其於中孔洞沸石中之限制生長
Chemical Vapor Deposition Synthesis Growth of Manganese-Doped and Spatially-Confined Perovskite Nanoparticles onto Mesoporous Zeolites
指導教授: 劉沂欣
Liu, Yi-Hsin
口試委員: 闕居振
Chueh, Chu-Chen
謝明惠
Shieh, Ming-Huey
口試日期: 2021/08/03
學位類別: 碩士
Master
系所名稱: 化學系
Department of Chemistry
論文出版年: 2021
畢業學年度: 109
語文別: 中文
論文頁數: 87
中文關鍵詞: 中孔洞沸石奈米粒子氧化石墨烯化學氣相沉積法二氧化碳還原
英文關鍵詞: mesoporous zeolite nanoparticles, graphene-oxide, chemical vapor deposition, CO2 reduction reaction
DOI URL: http://doi.org/10.6345/NTNU202101183
論文種類: 學術論文
相關次數: 點閱:112下載:10
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  • 本研究以高表面積(SBET > 800 m2 / g)的中孔沸石奈米粒子(mesoporous zeolite nanoparticles, MZNs)做為基材,於高溫下(700-900°C)溴化鉛與溴化銫為前驅物進行化學氣相沉積(chemical vapor deposition, CVD)反應,合成中孔洞限制的CsPbBr3/Cs4PrBr6的鈣鈦礦(pervoskite)奈米粒子。鈣鈦礦奈米粒子大小可以藉由前驅物比例及溫度改變加以調控,其電子結構及型貌利用紫外-可見光譜儀、螢光光譜儀、X-光繞射及穿透式電子顯微鏡佐證。合成過程中引入鎂離子及具有未成對電子的錳離子,使摻雜之鈣鈦礦奈米粒子放光具有不同波長,其結構組成、電子結構及自旋特性,以感應偶合電漿質譜、X光繞射光譜、螢光光譜及電子順磁共振光譜儀證實。此外,使用具半導體特性的中孔氧化石墨烯奈米粒子(mesoporous graphene-oxide nanoparticles, MGNs)做為基材時,可有效增進電荷分離效率,於照光下可使二氧化碳還原成一氧化碳,並以紫外-可見光譜儀及螢光光譜佐證其電子結構之變化。無機鈣鈦礦材料具良好的發光及催化效能,未來欲結合中孔洞薄膜材料之生長,生長具大氣穩定之太陽能轉換材料,提供異質結構於中孔洞沸石材料上限制生長之研究。

    In this study, mesoporous zeolite nanoparticles (MZNs) with high surface area (SBET>800 m2/g) was used as robust substrates to synthesize spatially confined CsPbBr3/Cs4PrBr6 (perovskite) nanoparticles (PV@MZNs) via chemical vapor deposition (CVD) at high temperature (700-900 °C) with two precursors, CsBr and PbBr2. The grain sizes of the perovskites were modulated by precursor ratios and reaction temperature. Ultraviolet-visible absorption spectroscopy (UV-Vis), fluorescence spectroscopy (FS), X-ray powder diffraction (XRD) and transmission electron microscopy (TEM) were utilized to characterize electronic structures and crystals of PV@MZNs. Magnesium and manganese ions were introduced to dope the perovskites, showing unique phosphorescence property. The characterizations of compositions, electronic and spin structures were assured by induced coupled plasma mass spectrometry, XRD, FS and electron paramagnetic resonance, individually. Moreover, heterostructures for PV@MZNs can be created when mesoporous graphene-oxide nanoparticles (MGNs) were introduced. Charge separation can be observed by fluorescence quenching and photocatalytic CO2 reductions into CO. Inorganic perovskite materials with excellent optical and catalytic performance, combined with mesoporous zeolite thin films (MZTFs) and heterostructures showing confined dimensions on silicon substrates, are rationally targeted for stable ambient solar energy converters.

    謝誌 i 摘要 ii Abstract iii 目錄 iv 圖目錄 vii 表目錄 x 第一章 緒論 1 1.1 鉛-鹵素鈣鈦礦材料概要 1 1.1.1 能系調控 2 1.1.2 維度調控 4 1.1.3 提升穩定度 5 1.1.3.1表面鈍化 6 1.1.3.2 鎂離子摻雜 8 1.2 光催化反應 9 1.2.1 粒徑調控 10 1.2.2 錳離子摻雜 11 1.2.3 異質結構 13 1.3 研究動機 15 第二章 實驗方法 16 2.1化學藥品 16 2.2中孔洞沸石奈米粒子 18 2.2.1 沸石晶種之合成 18 2.2.2 奈米粒子合成 19 2.2.3 石墨烯化中孔洞沸石奈米粒子 19 2.3 中孔洞沸石-鈣鈦礦複合材料 19 2.3.1 奈米粒子附載鈣鈦礦量子點 20 2.3.2 奈米粒子附載摻雜錳鈣鈦礦量子點 20 2.3.3奈米粒子附載摻雜鎂鈣鈦礦量子點 21 2.4 二氧化碳還原反應 21 2.5 實驗與鑑定裝置 22 2.5.1 穿透式電子顯微鏡 (TEM) 22 2.5.2 紫外-可見光光譜 (UV-Vis) 22 2.5.3 螢光光譜儀 (PL) 23 2.5.4 螢光量子產率分析儀 (QY) 24 2.5.5 物理吸脫附分析儀 (BET) 25 2.5.6 X 光粉末繞射儀 (PXRD) 26 2.5.7 熱重分析儀 (GA) 27 2.5.8電子順磁共振光譜 (EEPR) 28 2.5.9化學氣相沉積 (CVD) 29 2.5.10 感應耦合電漿質譜分析儀 (ICP-MS) 29 2.5.11氣相層析儀-阻擋放電離子化檢測器 (GC-BID) 30 2.6名稱縮寫統整 31 第三章 結果與討論 32 3.1 合成條件討論 32 3.1.1 載體熱穩定性探討 32 3.1.2 反應溫度 36 3.1.3 反應時間 43 3.2 能隙調控 49 3.2.1 前驅物比例影響 49 3.2.2 前驅物濃度影響 55 3.3 金屬離子摻雜 63 3.3.1 錳離子摻雜 63 3.3.2 鎂離子摻雜 69 3.4 奈米粒子表面修飾影響 75 第四章 結論 81 參考資料 82

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