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研究生： 吳冠賢
Wu, Kuan-Hsien
論文名稱： Cu2SnSe3和Cu2(Sn1-xInx)Se3奈米晶的熱溶合成及其性質研究
Solvothermal synthesis and properties of Cu2SnSe3 and Cu2(Sn1-xInx)Se3 nanocrystals
指導教授： 林文台
Lin, Wen-Tai
學位類別： 碩士
Master
系所名稱： 工學院 - 材料科學及工程學系
Department of Materials Science and Engineering
論文出版年： 2012
畢業學年度： 100
語文別： 中文
論文頁數： 117
中文關鍵詞： 熱溶法 、高壓釜 、Cu2SnSe3奈米晶 、Cu2(Sn1-xInx)Se3奈米晶
外文關鍵詞： solvothermal, autoclave, Cu2SnSe3 nanocrystals, Cu2(Sn1-xInx)Se3 nanocrystals
相關次數： 點閱：58  下載：1 
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    • 本論文藉由兩種熱溶法來合成Cu2SnSe3(CTSe)及In摻雜CTSe(CTISe)奈米晶，並探討不同溶劑、前驅溶液之莫耳配比、溫度、時間等對合成之影響，同時探討CTSe與In摻雜CTSe奈米晶之光學及熱電性值。於高壓釜中放入含有聯胺及乙二胺溶劑的前驅溶液，可加速CTSe及CTISe之合成。於高壓釜中在190ºC分別持溫48及72小時可合成出純相之CTSe與In摻雜CTSe奈米晶。其原因為聯胺具有使硫系金屬化合物於反應中降低維度(dimentional reduction)之功能。由於In摻雜的影響，CTISe之反應速率比CTSe慢。以油胺為溶劑的前驅溶液，於氮氣中在210ºC分別持溫36及60小時可合成出純相之CTSe與In摻雜CTSe奈米晶，其也顯示In摻雜會使CTSe奈米晶之反應速率變慢。In摻雜CTSe奈米晶之拉曼光譜圖於180cm-1之峰值比CTSe奈米晶之峰值寬，其顯示In摻雜後會導致CTSe之化學鍵結改變。CTSe及In摻雜CTSe奈米晶藉由UV-vis光譜儀所測得之能隙約為1.08 eV，其顯示In摻雜對CTSe之能隙無顯著影響。

    In the present study, the synthesis of Cu2SnSe3 (CTSe) and In-doped CTSe (CTISe) nanocrystals by two solvothermal processes as a function of the solvent, the molar ratio of precursors, temperature and time were explored. Meanwhile, the optical and thermoelectric properties of CTSe and CTISe nanocrystals were also studied. On synthesis in an autoclave, the addition of hydrazine to the ethylenediamine solvent speeded up the formation of pure CTSe and CTISe nanocrystals at 190˚C for 48 and 72 h, respectively. The reason can be explained in terms of the dimensional reduction of metal chalcogenides in the solvothermal reaction by hydrazine. However, as compared with the undoped CTSe nanocrystals, the formation rate of CTISe nanocrystals is significantly depressed due to In doping. On synthesis in N2 in the oleylamine solvent, the pure CTSe and CTISe nanocrystals could be acquired at 210˚C for 36 and 60 h, respectively, also revealing that In-doping depressed the growth rate of CTSe nanocrystals. The broader peak at 180 cm-1 in the Raman spectrum of CTISe nanocrystals as compared with that of CTSe nanocrystals indicates that the In-doping induces a change of the chemical bonding in the CTSe lattice. The bandgaps of CTSe and CTISe nanocrystals were determined to be about 1.08 eV by UV-vis spectroscopy, revealing that the In doping had no significant effect on the bandgap of the CTSe crystals.

    目錄 中文摘要 I Abstract II 誌謝 III 目錄 IV 圖目錄 VIII 第一章 引言 1 第二章 理論基礎與文獻回顧 3 2.1 熱電材料 3 2.1.1 Seebeck效應[7-9] 3 2.1.2 Peltier效應[10] 4 2.1.3 Thomson效應[11-15] 4 2.1.4 熱電優值[9, 16, 21] 5 2.1.5 熱電優值的發展歷史趨勢[21] 6 2.2 熱電材料的介紹 6 2.2.1 熱電材料物理特性需求 6 2.2.2 熱電材類分類 7 2.2.3 提升材料熱電優值的方法 8 2.3 CTSe文獻回顧 10 2.3.1 CTSe之結構 11 2.3.2 CTSe之熱電性質[1] 13 2.4 研究動機 16 第三章 實驗步驟與方法 19 3.1 以濕式化學法在高壓容器合成CTSe和CTISe粉末 19 3.1.1 合成CTSe粉末 19 3.1.2 合成CTISe粉末 20 3.2 以濕式化學法在氮氣合成CTSe和CTISe粉末 20 3.2.1 合成CTSe粉末 20 3.2.2 合成CTISe粉末 21 3.3 材料特性分析 21 3.3.1 X光繞射儀[61] 21 3.3.2 掃描式電子顯微鏡[61] 23 3.3.3 穿透式電子顯微鏡[61] 24 3.3.4 X光能量散佈分析儀[61] 25 3.3.5 化學分析電子光譜儀[62] 26 3.3.6 紫外/可見光光譜儀[63] 28 3.3.7 拉曼光譜儀[64-65] 29 3.3.8熱電性值分析 30 第四章 結果與討論 33 4.1 熱溶法在高壓釜(autoclave)中合成CTSe及CTISe奈米晶 33 4.1.1 添加聯胺對合成CTSe奈米晶之影響 33 4.1.2 添加聯胺對合成CTISe奈米晶之影響 35 4.1.3 聯胺促進CTSe及CTISe奈米晶合成之機制 38 4.2 在高壓釜中合成CTSe及CTISe奈米晶之特性分析 40 4.2.1 CTSe及CTISe之微結構及化學組成 40 4.2.2 CTSe及CTISe之紫外-可見光譜分析 41 4.3 熱溶法在氮氣中合成CTSe及CTISe奈米晶 42 4.3.1 合成CTSe奈米晶 42 4.3.2 合成CTISe奈米晶 44 4.4 在氮氣中合成CTSe及CTISe奈米晶之特性分析 46 4.4.1 CTSe及CTISe之微結構及成份分析 46 4.4.2 CTSe及CTISe之紫外-可見光譜分析 48 4.5 真空退火 48 4.5.1 用高壓釜製備CTSe及CTISe奈米晶之真空退火 48 第五章 結論 50 參考資料 52 附錄 111 JCPDS Cards No. 01-086-1239 (CuSe) 111 JCPDS Cards No. 01-072-8034 (Cu2SnSe3) 112 JCPDS Cards No. 01-072-7165 (Cu2Se) 114 JCPDS Cards No. 00-006-0362 (Se) 115 JCPDS Cards No. 00-048-1224 (SnSe) 116 JCPDS Cards No. 01-072-7165 (Cu2SnSe4) 117 圖目錄 圖1 Seebeck效應示意圖[9] 59 圖2 Peltier效應示意圖[9] 59 圖3 Thomson效應示意圖[9] 60 圖4 分析封閉熱電迴路中之熱現象[9] 60 圖5(a) 熱電優值的發展歷史趨勢[21] 61 圖5(b) 熱電優值的發展歷史趨勢[21] 61 圖6 電導率、Seebeck係數、功率因子和熱傳導率隨載子濃度變化的曲線圖[21] 62 圖7 各類材料熱電優值(Z)隨工作溫度變化圖[21] 62 圖8 理想的熱電材料其電子能帶結構[21] 63 圖9 載子密度過晶界能障前後變化之示意圖[29] 63 圖10 晶界能障對不同能量載子散射之示意圖 64 圖11 Cu2SnSe3之晶格結構[39] 64 圖12 skutterudite及filled skutterudite之晶格結構[28] 65 圖13 Cu2SnSe3在晶體面(100)面之上層價帶(大於0.3eV)部分載子密度分佈圖。[1] 65 圖14 Cu2ZnSnSe4在(100)面之上層價帶(大於0.3eV)部分載子密度分佈圖。[1] 66 圖15 各比例CTISe之XRD圖。[1] 66 圖16 Cu2Sn0.9275In0.0625Se3在(100)面之上層價帶(大於0.3eV)部分載子密度分佈圖。[1] 67 圖17 以熱溶法於高壓容器中合成CTSe及CTISe奈米晶之流程圖 68 圖18 以熱溶法於氮氣中合成CTSe和CTISe粉末之流程圖 69 圖19 高壓釜不鏽鋼外殼及內襯之照片 70 圖20 高壓釜鎖緊後之照片 71 圖21 架設氮氣後之示意圖 71 圖22 布拉格定律示意圖 72 圖23 不同光子散射過程躍遷能階圖[84] 72 圖24 Seebeck量測示意圖 73 圖25 四點探針量測示意圖 73 圖26 熱傳導量試片裝置意圖 73 圖27 不加聯胺於高壓釜中在190ºC持溫48小時合成CTSe之XRD及Raman圖 74 圖28 添加聯胺於高壓釜中在190ºC分別持溫24、36及48小時合成CTSe之XRD及Raman光譜圖 75 圖29 於高壓釜中合成純相之CTSe粉末的ESCA分析圖。 76 圖30 不加聯胺於高壓釜中在190ºC持溫72小時合成CTISe之XRD及Raman圖 77 圖31 添加聯胺於高壓釜中在190ºC持溫48、60及72小時合成CTISe之XRD及Raman光譜圖 78 圖32 於高壓釜中合成純相之CTISe之ESCA分析圖 79 圖33 於高壓釜中合成純相之CTSe及CTISe以矽基板校正後的XRD圖 80 圖34 維度隨MX3與AbX結合量增加而降低之示意圖[83] 81 圖35 有添加聯胺於高壓釜中以190ºC持溫48小時所得CTSe粉末之SEM照片 82 圖36 無添加聯胺於高壓釜中以190ºC持溫48小時所得CTSe之SEM照片 83 圖37 有添加聯胺於高壓釜中以190ºC持溫72小時所得CTISe粉末之SEM照片 84 圖38 無添加聯胺於高壓釜中以190ºC持溫48小時所得CTISe粉末之SEM照片 85 圖39 於高壓釜中合成純相之CTSe粉末及CTISe粉末之SEM/EDS能譜分析 86 圖40 於高壓釜中合成純相之CTISe粉末之FE-SEM/EDS能譜分析 86 圖41 於高壓釜中合成CTSe奈米晶之TEM影像分析圖 87 圖42 於高壓釜中合成CTISe奈米晶之TEM影像分析圖 87 圖43 於高壓釜中合成CTSe米晶之繞射圖及其d值。 88 圖44 於高壓釜中合成CTISe奈米晶之TEM繞射圖及其d值。 89 圖45 於高壓釜中合成CTSe粉末及CTISe粉末之SEM/EDS能譜分析 90 圖46 配比Cu2SnSe2於氮氣中在170ºC反應24小時合成CTSe之XRD圖及SEM/EDS分析結果。 90 圖47 配比Cu1.7SnSe2於氮氣中分別在在190、200及210ºC反應24小時合成CTSe之XRD圖及Raman光譜圖。 91 圖48 配比Cu1.7SnSe2於氮氣中分別在190、200及210ºC反應24小時合成粉末之SEM/EDS成份分析結果。 92 圖49 配比Cu1.7SnSe2於氮氣中在210ºC反應36及48小時合成CTSe之XRD圖及Raman光譜圖。 93 圖50 配比Cu1.5SnSe1.8於氮氣中在210ºC反應36小時合成CTSe之XRD圖及Raman光譜圖。 94 圖51 配比Cu1.7Sn0.8In0.2Se2於氮氣中在210ºC，分別反應36、48及60小時合成CTISe之XRD圖及Raman光譜圖。 95 圖52 配比Cu1.5Sn0.8In0.2Se1.8於氮氣中在210ºC，分別反應36、48及60小時合成CTISe之XRD圖及Raman光譜圖。 96 圖53 於氮氣中合成CTSe及CTISe以矽基板校正後之XRD圖 97 圖54 於氮氣中合成CTSe粉末之SEM照片。 98 圖55 於氮氣中CTISe粉末之SEM照片。 99 圖56 配比Cu1.7SnSe2於氮氣中合成CTSe及CTISe粉末之SEM/EDS能譜分析 100 圖57 配比Cu1.7SnSe2於氮氣中合成CTSe及CTISe奈米片狀之SEM/EDS能譜分析 100 圖58 於氮氣中配比Cu1.5SnSe1.8合成CTSe及CTISe粉末之SEM/EDS能譜分析 101 圖59 於氮氣中配比Cu1.5SnSe1.8合成CTSe及CTISe粉末奈米片狀之SEM/EDS能譜分析 101 圖60 於氮氣中CTSe奈米晶之TEM影像分析圖 102 圖61 於氮氣中CTISe奈米晶之TEM影像分析圖 102 圖62 於氮氣中CTSe奈米晶之繞射圖及其d值。 103 圖63 於氮氣中CTSe奈米晶之繞射圖及其d值。 104 圖64 於氮氣中CTISe奈米晶之繞射圖及其d值。 105 圖65 於氮氣中合成CTSe及CTISe之UV-vis光譜圖。 106 圖66 於高壓釜中製備CTSe及CTISe真空退火之XRD及Raman圖 107 圖67 於高壓釜中製備CTSe真空退火之SEM照片 108 圖68 熱溶法於高壓釜中製備CTISe真空退火之SEM照片 109 圖69 於高壓釜中製備CTSe及CTISe真空退火之SEM/EDS能譜分析 110

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