臺灣博碩士論文加值系統

本論文是研究一鍋法合成三元ZAIS/ZnS核殼量子點，二硫代胺基甲酸鹽分別與硝酸銀，硝酸銦、硝酸鋅成單一金屬前驅物，接著以油胺為溶劑與保護劑進行一鍋化合成。利用核磁共振氫譜、元素分析得產物鑑定與純度分析，利用可見光紫外光分光光譜儀及螢光光譜儀分析ZAIS/ZnS 核殼量子點光學性質，最後利用穿透式電子顯微鏡及元素分析鑑定了量子點的尺寸大小與晶型結構。本論文一系列合成結果顯示成功合出了具有不錯熱穩定性及量子產率的ZAIS/ZnS量子點。

This thesis reports the one-pot synthesis of ternary ZAIS/ZnS
core-shell quantum dots. Three metal precursor complexes were obtained firstly by the reactions of, silver, indium and zinc nitrates and dithiocarbamate. The ZAiS/Zns were obtained by the one-pot synthesis method by usingoleyamine as solvent and protective agent. The product identification and purity analysis were carried out by nuclear magnetic resonance spectroscopy and elemental analysis. The optical properties of ZAIS/ZnS core-shell quantum dots were analyzed by visible UV spectrophotometer and the fluorescence spectrometer. Finally, quantum dots were determined by transmission electron microscopy and elemental analysis to confirm the size and crystal structure. The results of this thesis show that ZAIS/ZnS quantum dots with good thermal stability and high quantum yield could be obtained by one-pot synthesis method successfully.

目錄
第一章緒論 1
1-1奈米材料之簡介 1
1-2量子點簡介 2
1-3 尺寸效應 2
1-4.量子侷限效應 (Quantum Confinement Effect) 3
1-5.文獻回顧 5
1-5.1 II-VI 族 5
1-5.2. I-III-VI 族量子點 7
1-6.研究動機 12
第二章 實驗研究 14
2-1實驗架構 14
2-1.1 量子點合成 14
2-1.2 量子點鑑定 15
2-1.3量子點膜 16
2-2 藥品、溶劑 17
2-3儀器 19
2-3.1 核磁共振儀 (Nuclear Magnetic Resonance Spectroscopy, NMR) 19
2-4.2螢光光譜儀 (Fluorescence Spectrophotometer，FL) 20
2-4.3 動態光散射儀 (Dynamic Light Scattering, DLS) 20
2-4.4 熱重分析儀 (Thermogravimetric analysis) 20
2-4.5 掃描式電子顯微鏡（Sacnning Electron Microscope, SEM） 21
2-4.6 元素分析儀（Elemental Analyzer，EA） 22
2-4.7 穿透式電子顯微鏡 (Transmission Electron Microscope) & EDS 22
2.4-8 離心機 23
第三章 實驗步驟 24
3-1 金屬錯合前驅物合成 24
3-1.1 Ag(I)xanthate [Ag(S2CN(C2H5)2] 之合成步驟 24
3-1.2 In(III) xanthate [In(S2CN(C2H5)2)3] 之合成步驟 25
3-1.3 Zn(II) xanthate [Zn(S2CN(C2H5)2)2] 之合成步驟 25
3-1.4 [(AgIn)xZn2(1-x)(S2CN(C2H5)2)4] 混合前驅物之合成步驟 26
3-2 ZAIS核量子點合成 26
3-2.1 混合前驅物合成ZAIS綠光核量子點 (油鍋合成法) 27
3-2.2 混合前驅物合成ZAIS紅光核量子點 (油鍋合成法) 27
3-2.3 單一前驅物核成ZAIS綠光核量子點 (油鍋合成法) 28
3-2.4 單一前驅物核成ZAIS紅光核量子點 (油鍋合成法) 28
3-2.5 單一前驅物核成ZAIS綠光核量子點 (加熱包合成法) 29
3-2.5 單一前驅物核成ZAIS紅光核量子點 (加熱包合成法) 29
3-3 ZAIS核量子點熱處理 30
3-3.1 混合前驅物ZAIS核量子點熱處理綠光、紅光 (油鍋合成法) 30
3-3.2 單一前驅物ZAIS核量子點熱處理綠光、紅光 (油鍋合成法) 30
3-3.3 單一前驅物ZAIS核量子點熱處理綠光、紅光 (加熱包合成法) 31
3-4 ZAIS /ZnS 核殼量子點合成 31
3-5 ZAIS/ZnS 核殼量子點成膜 32
3-5.1 綠光量子點配體置換 32
3-5.2 紅光量子點配體置換 32
3.5-3 綠光量子點成膜 33
3.5-4 紅光量子點成膜 33
第四章 結果與討論 34
4-1 ZAIS 量子點合成步驟 34
4-1.1 合成ZAIS 金屬前驅物的選擇與光譜判斷 34
4-1.2 合成ZAIS核混合金屬前驅物與單一金屬前驅物比較 39
4-1.3 油胺與辛胺的選擇 40
4-1.4 油胺對混合金屬前趨物之影響 42
4-1.5 ZAIS核之熱處理 42
4-1.6 ZAIS波長條件設計 42
4-1.7 ZAIS溫度與時間條件設計 44
4-1.8 ZAIS 熱處理及包殼之最佳條件 49
4-1.9 ZAIS/ZnS 之包殼條件設計 50
4-2 ZIAS量子點之大量製備 52
4-2.1 ZAIS 紅光量子點之熱裂解 52
4-2.2 ZAIS紅光大量製備之熱處理 53
4-2.3 ZAIS 綠光大量製備之熱裂解 56
4-2.4 ZAIS綠光大量製備之熱處理 58
4-2.5 ZAIS/ZnS 之包殼條件之討論 61
4-2.6 ZAIS/ZnS小量合成與大量合成之比較 64
4-3 合成ZAIS/ZnS油鍋與加熱包的比較 69
4-3.1 合成ZAIS 加熱包之熱處理 69
4-3.2 加熱包合成ZAIS/ZnS 之波長測試 73
4-4 ZAIS/ZnS 之結果分析 74
4-4.1 量子產率 74
4-4.2 量子點尺寸 75
4-4.3 ZAIS/ZnS之EDS元素分析結果 81
4-4.4 ZAIS/ZnS 量子點金屬含量 83
4-5 ZAIS/ZnS 量子點成膜 85
4-5.1 配體置換 85
4-5.2 量子點成膜 87
第五章 結論 89
參考文獻 90
 
圖目錄
圖1- 10D~3D 半導體及其吸收光譜示意圖 3
圖1- 2不同大小粒徑 CdSe/ZnS 量子點的螢光光譜波峰範圍 7
圖1- 3無鎘量子點 (AIS 、CuInS2)黃銅礦結構 9
圖1- 4注射螢光QDs負載的FA-SOC後荷瘤小鼠的圖像 9
圖1- 5不同大小粒徑 ZAIS/ZnS 量子點的能階變化及螢光圖像 9

圖3- 1Ag(I)xanthate [Ag(S2CN(C2H5)2]合成流程圖 24
圖3- 2In(III) xanthate [In(S2CN(C2H5)2)3] 合成流程圖 25
圖3- 3 Zn(II) xanthate [Zn(S2CN(C2H5)2)2] 合成流程圖 25

圖4- 1 混合金屬前驅物1H-NMR 35
圖4- 2 單一金屬前驅物 1H-NMR 疊圖 35
圖4- 3單一金屬前驅物Carbamate-Ag 元素分析圖譜 36
圖4- 4單一金屬前驅物Carbamate-In 元素分析圖譜 37
圖4- 5單一金屬前驅物Carbamate-Zn 元素分析圖譜 38
圖4- 6混合金屬前驅物熱裂解螢光光譜圖 40
圖4- 7單一金屬前驅物熱裂解螢光光譜圖 40
圖4- 8單一金屬熱裂解辛胺修飾表面之螢光光譜圖 41
圖4- 9不同金屬比例熱裂解的螢光放光光譜比較 43
圖4- 10綠光不同熱裂解溫度螢光放光光譜比較 45
圖4- 11紅光不同熱裂解溫度螢光放光光譜比較 46
圖4- 12綠光不同熱裂解時間螢光放光光譜比較 47
圖4- 13紅光不同熱裂解時間螢光放光光譜比較 48
圖4- 14熱處理後包殼與未熱處理後包殼的螢光放光光譜比較 49
圖4- 15不同鋅鹽類包殼螢光放光光譜比較 51
圖4- 16單一前驅物二重複合成ZAIS之熱裂解螢光光譜圖 52
圖4- 17混合前驅物二重複合成ZAIS之熱裂解螢光光譜圖 53
圖4- 18紅光大量製備熱處理溫度螢光放光光譜比較 54
圖4- 19紅光大量製備熱處理時間螢光放光光譜比較 55
圖4- 20綠光熱裂解二重複螢光光譜圖 56
圖4- 21ZAIS大量製備綠光最佳熱裂解溫度螢光光譜圖 57
圖4- 22綠光大量製備熱處理溫度螢光放光光譜比較 59
圖4- 23綠光大量製備熱處理時間螢光放光光譜比較 60
圖4- 24ZnS殼離心後的大顆粒 62
圖4- 25形成ZnS殼溶液狀態 62
圖4- 26ZAIS核包殼後 63
圖4- 27綠光熱裂解、熱處理、包殼後比較圖 63
圖4- 28紅光熱裂解、熱處理、熱處理包殼比較圖 64
圖4- 29綠光不同金屬比例比較 (小量) 65
圖4- 30紅光不同金屬比例比較 (小量) 66
圖4- 31綠光不同金屬比例比較 (大量) 67
圖4- 32紅光不同金屬比例比較 (大量) 68
圖4- 33加熱包160 oC熱處理時間螢光光譜 70
圖4- 34加熱包170 oC熱處理時間螢光光譜 71
圖4- 35加熱包190 oC熱處理時間螢光光譜 72
圖4- 36加熱包合成ZAIS/ZnS 不同當量比螢光光譜 73
圖4- 37量子產率 74
圖4- 38熱裂解之量子點平均粒徑分析 76
圖4- 39熱裂解之量子點粒徑分佈 76
圖4- 40熱處理之量子點平均粒徑分析 77
圖4- 41熱處理之量子點粒徑分佈 77
圖4- 42包殼後之量子點平均粒徑分析 78
圖4- 43包殼後之量子點粒徑分佈 78
圖4- 44綠光ZAIS/ZnS量子點之SEM 79
圖4- 45紅光ZAIS/ZnS量子點之SEM 79
圖4- 46綠光ZAIS/ZnS量子點之TEM QDs~2.5 80
圖4- 47紅光ZAIS/ZnS量子點之TEM QDs~3.0~3.5 80
圖4- 48綠光ZAIS/ZnS 量子點EDS元素分析 81
圖4- 49紅光ZAIS/ZnS 量子點EDS元素分析 82
圖4- 50純化一次後量子點之熱分析光譜 84
圖4- 51純化5次後量子點之熱分析光譜 84
圖4- 52ZAIS/ZnS與4種配體置換於甲苯溶劑中 86
圖4- 53ZAIS/ZnS與4種配體置換於甲苯溶劑中之螢光燈下 86
圖4- 54紅綠光ZAIS/ZnS配體製換 1H-NMR圖譜疊圖比較 87
圖4- 55ZAIS/ZnS綠光量子點膜405nm紫光照射下 88
圖4- 56ZAIS/ZnS紅光量子點膜405nm紫光照射下 88
圖4- 57綠光、紅光量子點成膜之固態PL之疊圖 88


表目錄
表1- 1近十年來的無鎘量子點研究報導文獻 10
表1- 2近年發展量子點的QY 11
表4- 1 單一金屬前驅物EA分析表 39
表4- 2 不同金屬比例熱裂解波峰與半波寬比較 43
表4- 3 綠光不同熱裂解溫度波峰、半高寬、放光強度比較 45
表4- 4 紅光不同熱裂解溫度波峰、半高寬、放光強度比較 46
表4- 5 綠光不同熱裂解時間波峰、半波寬、放光強度比較 47
表4- 6 紅光不同熱裂解時間波峰、半波寬、放光強度比較 48
表4- 7 不同實驗條件波峰、半波寬、放光強度比較 50
表4- 8 不同鋅鹽類包殼波峰、半波寬、放光強度比較 51
表4- 9 紅光大量製備熱處理溫度的波峰、半波寬、放光強度比較 54
表4- 10 紅光大量製備熱處理時間波峰、半波寬、放光強度比較 55
表4- 11 綠光大量製備熱裂解溫度波峰、半波寬、放光強度比較 57
表4- 12 綠光大量製備熱處理溫度的波峰、半波寬、放光強度比較 59
表4- 13 綠光大量製備熱處理時間波峰、半波寬、放光強度比較 60
表4- 14 近五年來以不同鋅鹽類包殼之無鎘量子點研究報導文獻 62
表4- 15 綠光ZAIS/ZnS不同金屬比例波長、半高寬、產率比較 65
表4- 16 紅光ZAIS/ZnS不同金屬比例波長、半高寬、產率比較 66
表4- 17 綠光ZAIS/ZnS不同金屬比例波長、半高寬、產率比較 67
表4- 18 紅光ZAIS/ZnS不同金屬比例波長、半高寬、產率比較 68
表4- 19 加熱包160 oC熱處理時間波峰、半波寬、放光強度比較 70
表4- 20 加熱包170 oC熱處理時間波峰、半波寬、放光強度比較 71
表4- 21 加熱包190 oC熱處理時間波峰、半波寬、放光強度比較 72
表4- 22 加熱包合成ZAIS/Zn不同金屬比例熱裂解波峰與半波寬比較 73

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