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研究生:謝佳倩
研究生(外文):Jia-Cian Hsieh
論文名稱:常壓電漿及水熱混成技術沉積三氧化鎢膜層於電致變色之應用研究
論文名稱(外文):Investigation of Electrochromic Properties of Novel Tungsten Trioxide Nano-structure Preparation Using Hydrothermal Process.
指導教授:劉文仁劉文仁引用關係
指導教授(外文):Wen-Jen Liu
學位類別:碩士
校院名稱:義守大學
系所名稱:材料科學與工程學系
學門:工程學門
學類:材料工程學類
論文種類:學術論文
論文出版年:2016
畢業學年度:104
語文別:中文
論文頁數:266
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本研究目的為利用種晶層輔助水熱法製備一維方向生長之六方晶體三氧化鎢奈米棒薄膜結構,應用於電致變色元件之變色層,並探討其微觀表面型態與電致變色元件之光學與化學性質測試。種晶層部分分別為利用旋鍍法將鎢酸溶液鍍於FTO玻璃基板上製備所需之種晶層,以及藉由本實驗自行開發之常壓電漿噴流(Atmospheric Pressure Plasma Jet)金屬電極沉積系統於FTO玻璃基板上製備種晶層。將已鍍有種晶層之FTO基板置入由鎢酸鈉(Sodium tungstate, Na2WO4)、鹽酸(Hydrochloric acid, HCl)、草酸(Oxalic acid, H2C2O4)及醋酸鈉(Sodium acetate, CH3COONa)所調配之水熱前驅溶液中,透過此四種藥品之濃度參數、水熱反應之溫度及時間的改變進行實驗,成長六方晶結構(Hexagonal structure)之三氧化鎢變色層膜層。在經過一系列研究中發現,於FTO玻璃基板上製備三氧化鎢膜層之最佳實驗參數為使用電漿沉積種晶層,採用水熱前驅液為鎢酸鈉濃度0.25M、PH值2.2、包覆劑濃度0.0075mol,成長溫度為190℃、時間為2小時。最佳實驗參數試片呈現最佳電致變色特性,主要為具備高比表面積及多孔結構,利於電解液中之鋰離子進行反應;同時,經由循環伏安2000次循環測試結果顯示穩定性相當優異。

The purpose of this study is to fabricate the one-dimension tungsten trioxide (WO3) nano-rod (WNRs) films by hydrothermal process and investigate the relationship between microstructure morphologies and electrochromic properties. A WO3 seed layer with monoclinic structure was deposited on a fluorine doped tin oxide (FTO) coated glass substrate by spin coating and atmospheric pressure plasma jet deposition system. The mixtures of sodium tungstate (Na2WO4), hydrochloric acid (HCl), oxalic acid (H2C2O4) and sodium acetate (CH3COONa, capping agent) were adopted to be the precursors of WO3 films for the hydrothermal process. By a series of experiments, it was found the optimal process parameters for synthesizing WO3 films on FTO substrates were seed layer prepared by atmospheric plasma and the hydrothermal precursors using Na2WO4 concentration of 0.25M, the pH of 2.2, the capping agent of 0.0075mol, the growth temperature of 190oC and the growth time of 2 hr. It revealed the optimal process parameters samples possessed best electrochromic properties is due to having high specific surface area and porous structure which resulted in more easily react with lithium ion (Li+) in the electrolyte. Meanwhile, the optimal process parameters samples also revealed very good reliability from the 2000 cycles of cyclic voltammetry (CV) test.

中文摘要 I
英文摘要 III
誌謝 IV
總目錄 VI
表目錄 VIII
圖目錄 XI
第一章 緒論 1
1-1 前言 1
1-2 實驗動機與目的 5
第二章 理論基礎 7
2-1 智慧變色材料之種類 7
2-2 電致變色材料之種類[11] 12
2-3 電致變色元件之原理[16] 18
2-4 電致變色元件的種類 19
2-5 三氧化鎢之簡介 23
2-6 非晶之氧化鎢電致變色機制 27
2-7 結晶氧化鎢之電致變色機制 30
2-8 電漿基本原理 32
2-9 電漿之種類 42
2-10 水熱法 48
2-11 奈米材料之簡介[48] 49
2-12 一維奈米尺寸材料之優勢 53
第三章 文獻回顧 54
3-1 水熱製程之文獻 55
3-2 常壓電漿製程之文獻 74
3-3 熱絲化學氣相沉積法(Hot-wire chemical vapor deposition, HWCVD 76
3-4 溶膠-凝膠法(Sol-Gel)78
第四章 實驗製程 80
4-1 實驗材料與設備 80
4-2 實驗流程 83
4-3 分析與量測之儀器 95
4-4 電致變色薄膜性質之探討[84] 101
第五章 實驗結果與討論 108
5-1 旋鍍法製備三氧化鎢種晶層之膜層 110
5-2 旋鍍種晶層輔助水熱法生長三氧化鎢奈米棒 114
5-3 常壓電漿製備三氧化鎢種晶層之膜層 132
5-4 常壓電漿製備種晶層輔助水熱法生長三氧化鎢奈米棒 146
5-5 種晶層輔助水熱成長之最佳參數TEM結構分析 164
5-6 三氧化鎢薄膜之電致變色性質探討 172
5-7 常壓電漿輔助水熱法成長三氧化鎢奈米棒膜層之XPS分析 195
5-8 玻璃電極沉積非晶質之氧化鎢膜層 197
第六章 結論 221
第七章 未來努力方向 223
參考文獻 224

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