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研究生: 朱家慶
Chu, Chia-Ching
論文名稱: 氣態氘化鈉分子X-A的激發光譜研究和硫化鋅奈米粒子的合成研究
The Excitation Spectroscopy of the NaD X-A Transitions and the Synthesis of ZnS Nanoparticles
指導教授: 黃守仁
Whang, Thou-Jen
學位類別: 碩士
Master
系所名稱: 理學院 - 化學系
Department of Chemistry
論文出版年: 2011
畢業學年度: 99
語文別: 中文
論文頁數: 103
中文關鍵詞: 氘化鈉雷射光譜激發光譜硫化鋅奈米粒子
外文關鍵詞: NaD, Laser spectroscopy, Excitation spectroscopy, Zinc sulfide, Nano particles
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  • Part I 氣態氘化鈉分子X-A的激發光譜研究
      在本實驗中,利用一道染料雷射光偵測氘化鈉(NaD)分子的A1Σ+激發光譜,並觀測到共75個激發光譜訊號,此外利用實驗數據推測得A1Σ+能態位能曲線谷底能量(Te)約為22703.976 cm-1。
      在計算工作方面,對於氘化鈉分子的X1Σ+能態躍遷到A1Σ+能態(v'=0-25, J'=0-15)有較完整的計算,並且將計算數值與實驗數值做比較;對於其量子能態的熱分布也做了相關的計算;最後還有法蘭克-康登因子的計算,包含該躍遷的波長數據等。

    Part II 硫化鋅奈米粒子的合成研究
      本實驗嘗試五種硫離子源來合成硫化鋅粒子,分別是硫脲、過硫酸銨、硫代硫酸鈉、硫氰酸鉀和硫化鈉,並使用硫酸鋅作為鋅離子來源。採用的合成方法為化學沉澱法,結果顯示硫脲、硫代硫酸鈉和硫化鈉是可以成功合成硫化鋅的,此外再以這三種化合物做延伸的實驗。在硫脲部分嘗試了三種不同的溶劑、改變不同反應濃度和添加不同比例的保護劑等實驗,可以合成出球狀且粒徑約150-200 nm的硫化鋅粒子。在硫代硫酸鈉的部分嘗試了兩種不同的溶劑、改變不同反應濃度和添加不同比例的保護劑等實驗,相同的也可以合成出球狀且粒徑約150-200 nm的硫化鋅粒子。然而在硫化鈉部份的結果就沒這麼理想,合成出的硫化鋅並非球狀,且粒徑分析與實驗條件的相關性並不高。實驗合成的硫化鋅粒子再利用XRD鑑定後可以確認使用硫脲合成的結果是具有少量的纖維鋅礦結構,主要還是以閃鋅礦結構所構成;而在硫代硫酸鈉和硫化鈉合成的結果顯示以閃鋅礦結構為主。

    Part I The Excitation Spectroscopy of the NaD X-A Transitions
    In this study, we used a UV dye laser to observe the A1Σ+ excitation spectrum of the sodium deuterium molecules (NaD), and had observed all over 75 excitation signals. Furthermore, we used experimental data to infer that the energy at the bottom of potential energy curve (Te) of A1Σ+ is about 22703.976 cm-1.
    In the calculation works, we had done a more complete calculation about the sodium deuterium molecules, X1Σ+ A1Σ+ (v'=0-25, J'=0-15) transition, and compared with the experimental data. Also, we had carried out the thermal distribution of quantum states of the sodium deuterium molecules. Finally, we had calculated the Franck-Condon factors, including the wavelength of each transition.

    Part II The Synthesis of ZnS Nanoparticles
    In this study, we had tried five kinds of sulfide sources, thiourea, ammonium persulfate, sodium thiosulphate, potassium thiocyanate, and sodium sulfide respectively, and then used zinc sulfate as the source of zinc ion. The synthesis method we chose was chemical precipitation method, and the experimental results reveal that using thiourea, sodium thiosulphate, and sodium sulfide can synthesize zinc sulfide successfully. Moreover, we used these three kinds of compounds to do further experiments. In the thiourea part, we had tried three kinds of solvents, changed different reaction concentrations, and added different ratio of protection agent, and can synthesize spherical zinc sulfide, whose particle size is about 150-200 nm. In the sodium thiosulphate part, we also tried three kinds of solvents, changed different reaction concentrations, and added different ratio of protection agent, and, similarly, can synthesize spherical zinc sulfide, whose particle size is about 150-200 nm as well. However, in the sodium sulfide part, the result is not ideal. The zinc sulfide particles are not sphericity, and the particle size analysis results are not quite correlated with the experimental conditions. Finally, we made use of XRD to identify the structures of zinc sulfide. The structure of the zinc sulfide, synthesized by thiourea, is formed with small parts of wurtzite and major parts of sphalerite. The structure of the zinc sulfide synthesized by sodium thiosulphate and sodium sulfide chiefly belong to sphalerite.

    Part I 氣態氘化鈉分子X-A的激發光譜研究的中、英文摘要I Part II硫化鋅奈米粒子的合成研究的中、英文摘要II 誌謝III 目錄IV 表目錄VIII 圖目錄IX Part I 氣態氘化鈉分子X-A的激發光譜研究 第一章 緒論 1 1-1 前言 1 1-2 文獻回顧 3 第二章 理論 5 2-1 薛丁格方程式 5 2-2 波恩-奧本海默近似法 5 2-3 分子轉動光譜 6 2-4 分子振動光譜 7 2-5 雙原子分子振動轉動光譜 8 2-6 雙原子分子的電子態項符 9 2-7 躍遷選擇律 9 2-8 法蘭克-康登原理 10 2-9 同位素位移 10 第三章 實驗 12 3-1 實驗裝置 12 3-1-1 雷射系統 12 3-1-2 熱管爐系統 12 3-1-3 訊號偵測、收集與處理 13 3-2 實驗藥品 14 3-3 實驗介紹 15 第四章 結果與討論 18 4-1 雷射校正─中空陰極管 18 4-2 雷射校正─碘槽 20 4-3 NaD分子存在的確認與激發光譜 21 4-4 NaD分子的A1Σ+能態躍遷計算 26 4-5 NaD分子的量子能態的熱分布計算 27 第五章 結論 30 Part II 硫化鋅奈米粒子的合成研究 第一章 緒論 31 1-1 前言 31 1-2 文獻回顧 31 1-2-1硫化鋅型螢光體發展歷史 31 1-2-2 硫化鋅之晶體結構 32 1-2-3 硫化鋅之性質與應用 33 第二章 理論 34 2-1 發光中心之種類與原理 34 2-1-1 發光中心(luminescence center)發光 34 2-1-2 螢光主體(host)發光 35 2-2 奈米粒子簡介 36 2-3 螢光體製程技術與原理 37 2-3-1 固態燒結法 37 2-3-2 共沉澱法 37 2-3-3 水熱法 37 2-3-4 溶膠-凝膠法 37 2-3-5 化學沉澱法 38 2-3-6 種晶助熔法 38 2-4 化合物釋放硫的特性與奈米粒子抑制聚集簡述 38 第三章 實驗 39 3-1 實驗分析儀器 39 3-1-1 高解析掃描式電子顯微鏡及能量散佈分析儀 39 3-1-2 粒徑分析儀 39 3-1-3 X光粉末繞射儀 39 3-2 實驗裝置 39 3-3 實驗藥品 40 3-4 實驗介紹 41 3-4-1 硫脲與硫代硫酸鈉的實驗部份 42 3-4-2 硫化鈉的實驗部份 42 3-4-3 產物後續處理 42 第四章 結果與討論 43 4-1 硫離子來源選擇 43 4-2 硫脲 43 4-2-1 以去離子水做為溶劑 44 4-2-2 以甲醇/去離子水(1:3)做為溶劑 47 4-2-3 以甲醇/去離子水/乙二醇(1:3:1)做為溶劑 49 4-3 硫代硫酸鈉 51 4-3-1 以去離子水做為溶劑 51 4-3-2 以甲醇/去離子水(1:3)做為溶劑 56 4-4 硫化鈉 61 4-4-1 以去離子水做為溶劑 61 4-4-2以甲醇/去離子水(1:3)做為溶劑 62 4-5 XRD分析 63 第五章 結論 66 參考文獻 68 附錄 71 附錄A 72 附錄B 98 附錄C 101

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