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研究生： 黃國綸
Huang, Guo-Lun
論文名稱： 以硼氫化鈉活化備製錳摻雜硒化鎘團簇物及鑑定
Synthesis and Characterizations of Mn-doped (CdSe)13 Activated by NaBH4
指導教授： 劉沂欣
Liu, Yi-Hsin
口試委員： 李祐慈 黃信炅 劉沂欣
口試日期： 2021/09/28
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： 96
中文關鍵詞： 零維結構 、硒化鎘 、稀磁性半導體 、模板法 、中孔洞沸石材料 、魔術尺寸團簇物
英文關鍵詞： zero-dimension, cadmium selenide, diluted magnetic semiconductors, template, mesoporous zeolite nanoparticles, magic-size clusters
研究方法: 實驗設計法 、 主題分析
DOI URL： http://doi.org/10.6345/NTNU202101672
論文種類： 學術論文
相關次數： 點閱：98  下載：6 
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    • 本研究第一部份利用過去魔術尺寸硒化鎘奈米團簇物之合成方式，並以元素硒粉末代替價格昂貴的硒脲作為合成之前驅物在室溫下進行合成，透過紫外光-可見光譜儀、X光粉末繞射儀、元素分析以及固態核磁共振光譜儀，證實其同樣為雙生團簇物之結構。後續引入具有未成對電子的過度金屬錳離子，作為光學與磁性之改質，藉由穿透式電子顯微鏡、X光粉末繞射、可見光光譜儀、螢光光譜儀、X光吸收光譜延伸精細結構、電子順磁共振光譜儀、超導量子干涉儀以及磁圓偏振二色性光譜，確認形貌、晶體與電子結構、化學配位環境、未成對電子的存在，並探討錳摻雜之奈米團簇物之磁性性質與磁光性質的改變。
    我們在錳摻雜之奈米團簇物觀察到了反鐵磁性，在第二部分以高表面積之中孔洞沸石奈米粒子 (mesoporous zeolite nanoparticles, MZNs) 做為硬模板，在吸附[(CdSe)13]2限制奈米團簇物生長的同時，也試著分散具有磁性錳離子，藉由孔洞材料高介電的性質，改善錳-錳之間自旋的耦合作用。此外，中孔氧化石墨烯奈米粒子 (mesoporous graphene-oxide nanoparticles, MGNs) 做為模板時可增進導電性，未來欲結合中孔洞薄膜材料的生長，進行鑑定探討及討探索於稀磁性半導體之應用可能性。

    In this study, we use selenium powder instead of expensive selenourea as the precursor to synthesize (CdSe)13 nanoclusters at room temperature. Ultraviolet-visible absorption spectroscopy (UV-vis), elemental analysis (EA) and solid-state nuclear magnetic resonance spectroscopy (ssNMR) confirmed that it is also the twin clusters. Magnesium ions were introduced to dope the clusters, showing unique phosphorescence, magneto optical and magnetic properties. The characterizations of compositions, electronic and spin structure were assured by UV-vis, X-ray powder diffraction (XRD), infrared spectroscopy (IR), extended X-ray absorption fine structure (EXAFS), electron paramagnetic resonance, magnetic circular dichroism spectrophotometer (MCD) and superconducting quantum interference device magnetometer (SQUID).
    We have observed anti-ferromagnetism in Mn-doped (CdSe)13. In the second part, mesoporous zeolite nanoparticles (MZNs) with high surface area were used as hard templates to adsorb (CdSe)13, while limiting the growth of clusters, we also try to disperse magnetic manganese ions. In addition, Mn-doped (CdSe)13@MZNs can be created when mesoporous graphene-oxide nanoparticles (MGNs) were introduced. Charge separation can be observed by fluorescence quenching. Mn-doped (CdSe)13 combined with MGN show great candidate for catalytic applications.

    謝誌 i 摘要 ii Abstract iii 目錄 iv 圖索引 viii 表索引 xii 第一章 緒論 - 1 - 1.1 稀磁性半導體之概要 - 1 - 1.1.1 磁性記憶體之發展 - 2 - 1.1.2 稀磁性半導體面臨之挑戰 - 5 - 1.2 零維奈米團簇物 - 6 - 1.3 錳摻雜之零維團簇物 - 10 - 1.4 自旋-自旋耦合 - 14 - 1.4.1 孔洞材料之耦合調控 - 16 - 1.5 研究動機 - 17 - 第二章 實驗方法 - 18 - 2.1 化學藥品 - 18 - 2.2 雙生(CdSe)13奈米團簇物之合成 - 19 - 2.2.1 硒前驅物 - 19 - 2.2.2 鎘前驅物 - 19 - 2.2.3 硒化鎘奈米團簇物 - 20 - 2.3 合成摻雜錳之硒化鎘奈米團簇物 - 21 - 2.4 中孔洞材料內生長(CdSe)13 - 23 - 2.5 儀器鑑定 - 24 - 2.5.1 穿透式電子顯微鏡 ( TEM ) - 24 - 2.5.2 掃描式電子顯微鏡 ( SEM ) - 24 - 2.5.3 場發射掃描穿透式球差修正電子顯微鏡 ( HRTEM ) - 24 - 2.5.4 紫外-可見光吸收光譜儀 ( UV-vis ) - 25 - 2.5.5 螢光光譜儀 ( PL ) - 25 - 2.5.6 紅外光譜儀 ( FT-IR ) - 25 - 2.5.7 X光粉末繞射儀 ( PXRDs ) - 25 - 2.5.8 X光吸收光譜-吸收X光延伸精細結構 ( EXAFS ) - 26 - 2.5.9 元素分析儀 ( EA ) - 27 - 2.5.10 固態核磁共振儀及魔術角度旋轉技術 ( ssNMR ) - 27 - 2.5.11 交叉極化與異核交聯感應技術 ( CP, HETCOR ) - 27 - 2.5.12 電子順磁共振光譜儀 ( EPR ) - 28 - 2.5.13 磁圓偏振二色性光譜儀 ( MCD ) - 28 - 2.5.14 超導量子干涉磁量儀 ( SQUID ) - 29 - 2.5.15 感應耦合電漿放射光譜儀 ( ICP-OES ) - 30 - 第三章 結果與討論 - 31 - 3.1 前驅物對團簇物合成之影響與探討 - 31 - 3.1.1 硒先驅物之比較 - 31 - 3.1.2 團簇物形貌 - 32 - 3.1.3 團簇物尺寸及晶型 - 34 - 3.1.4 元素組成 - 37 - 3.1.5 化學配位環境 - 40 - 3.1.6 電子結構與能隙 - 46 - 3.2錳摻雜團簇物之鑑定與性質探討 - 48 - 3.2.1 元素組成 - 48 - 3.2.2 團簇物形貌 - 50 - 3.2.3 晶格收縮 - 51 - 3.2.4 化學配位環境 - 53 - 3.2.5 DFT理論計算 - 57 - 3.2.6 電子結構與能隙 - 58 - 3.2.7 摻雜對能隙之影響 - 61 - 3.3 硒化鎘團簇物之磁性探討 - 63 - 3.3.1 自旋光譜 - 63 - 3.3.2 磁光躍遷 - 67 - 3.3.3 逆磁性特徵 - 72 - 3.3.4 鐵磁性與超順磁性特徵 - 76 - 3.3.5 反鐵磁性特徵 - 78 - 3.3.6 巨大有效磁矩 (自旋極化) - 79 - 3.4 空間限制團簇物之生長 - 80 - 3.4.1 前驅物濃度效應 - 80 - 3.4.2 載體表面修飾 - 84 - 3.4.3 電子結構與能隙 - 87 - 第四章 結論 - 90 - 參考資料 - 91 -

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