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研究生:張翔
研究生(外文):Hsiang Chang
論文名稱:以草酸鋅為前驅物成長氧化鋅一維材料
論文名稱(外文):Synthesis of One-Dimensional Zinc Oxide from a Zinc Oxalate Precursor
指導教授:鄭如茵郭東昊
指導教授(外文):Ju-Yin ChengDong-Hau Kuo
學位類別:碩士
校院名稱:國立臺灣科技大學
系所名稱:工程技術研究所
學門:工程學門
學類:綜合工程學類
論文種類:學術論文
論文出版年:2010
畢業學年度:98
語文別:中文
論文頁數:127
中文關鍵詞:草酸鋅水溶液法退火一維氧化鋅材料
外文關鍵詞:zinc oxalateaqueous solution methodannealing processone-dimension ZnO materials
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本論文主要是使用草酸鋅為前驅物來成長氧化鋅一維材料,並討論在不同溫度、時間、模板比例、鹼性溶劑的量以及退火溫度等條件下對氧化鋅一維材料成長之影響。氧化鋅一維材料的水溶液法製備方式主要分為兩個步驟,首先利用氨水與草酸鋅分子反應形成錯離子後藉由HMTA的輔助來重新排列成一維的型態;第二步驟則是將前一步驟的產物經過不同溫度的退火處理來得到一維氧化鋅材料。
在實驗過程中,我們透過改變各種參數來討論氧化鋅一維材料的成長情況,並發現在HMTA對ZnC2O4的mole比為1:1、反應溫度80°C、反應時間30分鐘、NH4OH體積2ml、450°C退火30分鐘等條件下可以成長出長度45μm、直徑100~250nm的多晶氧化鋅一維材料,並輔以SEM顯微分析說明各種實驗參數不同的成長情況、TEM影像了解更細微的顯微結構、XRD分析鑑定產物組成、TGA得到退火熱裂解溫度、EDS及IR光譜來檢驗一維材料的成分以及透過UV-visible吸收光譜計算出產物的能帶間隙。
One-dimensional zinc oxide materials were prepared from commercially available zinc oxalate precursors. The effects of reaction temperature, reaction time, ratio of zinc oxalate and HMTA (hexamethylenetetramine), the concentration of the basic agent, and the annealing temperature on the preparation of one-dimensional (1-D) ZnO by an aqueous solution method were investigated. The formation of 1-D ZnO involved two steps. The first step was the dissolution of zinc oxalate by the solvent of ammonia to form the stable complexes. HMTA had already been incorporated into this solution to assist the zinc precursors in arranging into the 1-D configuration. At the second one, the products in the first step were annealed at different temperatures to obtain 1-D ZnO.
The experimental results demonstrate that the 1-D ZnO with the lengths of 45 μm and diameters of 100~250 nm have been produced with the conditions of the HMTA: ZnC2O4 ratio of 1:1, reaction temperature of 80°C, reaction time of 30 min, the ammonia aqueous solution of 2 ml, and annealing at 450°C for 30 min. SEM and TEM were used to observe the microstructure of 1-D materials grown at different conditions. The structure of the products was identified by X-ray diffraction. To ensure the thermal decomposition temperature, the TGA analysis was executed. EDS equipped on SEM and the IR spectroscopy were used to analyze the product composition. Energy gap of 450°C-annealed ZnO was calculated from the UV-vis data.
致謝 I
摘要 II
Abstract III
目錄 V
圖目錄 VIII
表目錄 XXII
第一章 導論 1
第二章 文獻回顧 6
2-1氧化鋅的晶體結構 6
2-2氧化鋅的發光性質 7
2-3氧化鋅一維奈米線製備方法 8
2-4氧化鋅一維奈米線成長機制 18
2-4-1溶劑的選擇對於成長氧化鋅一維奈米線的影響 24
2-4-2 pH值的控制對於成長氧化鋅一維奈米線的影響 26
2-4-3模板的輔助對於成長氧化鋅一維奈米線的影響 28
2-5摻雜對氧化鋅晶體放光的影響 37
2-6氧化鋅一維奈米線的應用 44
第三章 研究動機與實驗方法 53
3-1研究動機 53
3-2實驗方法 54
3-2-1實驗藥品與儀器 54
3-2-2實驗步驟 56
3-3儀器分析介紹 59
3-3-1掃描式/穿透式電子顯微鏡(SEM /TEM) 59
3-3-2 X光粉末繞射儀系統(X-Ray Diffractometer) 60
3-3-3 EDS/WDS成分分析 60
3-3-4紫外光/可見光光譜儀(UV-vis spectroscopy) 61
3-3-5傅立葉紅外線光譜儀(Fourier Transform Infrared Spectrometer) 61
3-3-6熱重損失分析儀(Thermogravimetric analysis, TGA) 62
第四章 結果與討論 63
4-1氨水濃度對於成長一維氧化鋅材料的影響 64
4-2不同HMTA與ZnC2O4的莫耳比對成長一維氧化鋅材料的影響 75
4-3不同濃度的ZnC2O4對成長一維氧化鋅材料的影響 81
4-4不同成長溫度對一維氧化鋅材料的影響 85
4-5化學物種添加方式與退火處理對成長一維氧化鋅材料的影響 98
4-6 TGA結果與分析 104
4-7 XRD結構分析 106
4-8 FT-IR分析 112
4-9 TEM顯微結構分析 113
4-10 UV-VIS分析 117
第五章 結論 120
參考文獻 121
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