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研究生:曹長安
研究生(外文):Chang-An Tsao
論文名稱:氧化鋅奈米線輔助電沉積法成長氧化鎢薄膜之電致色變性質研究
論文名稱(外文):Fabrication of electrochromic tungsten oxide thin film by electrodeposition method assisted with zinc oxide nanwires
指導教授:程金保程金保引用關係黃柏仁黃柏仁引用關係
指導教授(外文):Chin-Pao ChengBohr-Ran Huang
學位類別:碩士
校院名稱:國立臺灣師範大學
系所名稱:機電科技研究所
學門:工程學門
學類:機械工程學類
論文種類:學術論文
論文出版年:2011
畢業學年度:100
語文別:中文
論文頁數:85
中文關鍵詞:氧化鎢薄膜電致色變電沉積法氧化鋅奈米線
外文關鍵詞:tungsten oxide filmelectrochromicelectrodepositionzinc oxide nanowires
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本研究以電沉積法製備氧化鎢電致色變層,並輔以氧化鋅奈米線,應用於電致色變元件。本實驗分五部份進行,第一部份為使用定電流法沉積氧化鎢薄膜,第二部分使用定電壓法沉積氧化鎢薄膜,第三部分探討不同沉積時間對氧化鎢薄膜的影響。第四部份將試片去做退火熱處理,觀察結晶對電致色變性質的影響。最後部份為成長氧化鋅奈米線,先以濺鍍法在基板上沉積一層摻鋁的氧化鋅薄膜作為種子層,再以水熱法成長氧化鋅奈米線。將不同條件下成長的氧化鋅奈米線以穿透式電子顯微鏡觀察其表面形貌,再量測其穿透率,其穿透率隨成長時間上升而下降,成長15分鐘的氧化鋅奈米線穿透率已下降到70%。最後在不同基板上成長氧化鋅奈米線,以電沉積法在其上方沉積氧化鎢薄膜,觀察氧化鋅奈米線與電致色變的相關性。定電壓法沉積出之薄膜較定電流厚,退火後會使電致色變效果變差。沉積在摻鋁氧化鋅奈米線上的薄膜有最佳的電致色變性質,其著色效率可達15.40 cm2/C。
Electrodeposition method to fabricate WO3 electrochromic film which assisted with zinc oxide nanwire is used in this study. This study can be divided into five part. First, used constant current method to deposit WO3 film. Second, used constant voltage method to deposite WO3 film. Third, made different deposition time of WO3 film. Fourth, treated sample by annealing, and to observe the effect of electrochromic about crystal. Finally, grow AZO nanowires on the sputtering AZO film as seed layer by hydrothermal method. The microstructure and measurement transmittance of different AZO nanowires is observed by SEM. The transmittance decrease with the growing time increased. The transmittance decrease to 70% of AZO nanowires growing for 15 minute. The thickness of WO3 film by constant voltage is more large than constant current. Annealing will decrease the electrochromic effect. The film which deposit on AZO nanowise has the best electrochromic effect, the coloration efficiency can arrive 15.40 cm2/C.
目錄
第一章 序論.......................................1
1.1 研究背景..................................1
1.2 研究動機與目的..........................3
第二章 文獻回顧...............................................................................................5
2.1 電致色變元件..........................................................................................5
2.2 電致色變材料..........................................................................................7
2.3 電致色變機制........................................................................................10
2.4 電致色變層製備方法............................................................................12
2.5 電沉積法製備氧化鎢薄膜....................................................................14
2.6 水熱法成長氧化鋅奈米線....................................................................18
第三章 實驗方法與步驟.................................................................................24
3.1實驗藥品與耗材.....................................................................................24
3.2實驗流程規劃.........................................................................................25
3.2.1 電沉積法鍍液製備.........................................................................26
3.2.2 試片清洗.........................................................................................27
3.2.3 電沉積法製備氧化鎢電致色層.....................................................27
3.2.4 水熱法成長氧化鋅奈米線….........................................................28
3.2.5 電解液調配.....................................................................................30
3.3特性分析.................................................................................................31
3.3.1薄膜表面及微結構分析..................................................................31
3.3.2 X-ray繞射分析................................................................................31
3.3.3電化學分析......................................................................................31
3.3.4光學性質量測..................................................................................32
第四章結果與討論...........................................................................................33
4.1 定電流法沉積氧化鎢薄膜..................................................................33
4.1.1 SEM表面形貌分析.........................................................................33
4.1.2 AFM分析………............................................................................35
4.1.3 循環伏安法分析.............................................................................37
4.1.4 光學性質分析.................................................................................39
4.2 定電壓法沉積氧化鎢薄膜..................................................................43
4.2.1 SEM表面形貌分析.........................................................................43
4.2.2 AFM分析….……............................................................................45
4.2.3循環伏安法分析..............................................................................47
4.2.4光學性質分析..................................................................................48
4.3 不同沉積時間對氧化鎢薄膜的影響..................................................51
4.3.1 SEM表面形貌分析.........................................................................51
4.3.2 AFM分析…………….....................................................................54
4.3.3 循環伏安法分析.............................................................................56
4.3.4 光學性質分析.................................................................................57
4.4 退火熱處理..........................................................................................61
4.4.1 SEM表面形貌分析........................................................................61
4.4.2 AFM分析……………....................................................................62
4.4.3 XRD薄膜晶體結構分析................................................................64
4.4.4循環伏安法分析.............................................................................66
4.4.5光學性質分析.................................................................................67
4.5 氧化鋅奈米線......................................................................................69
4.5.1 SEM表面形貌分析........................................................................69
4.5.2 XRD薄膜晶體結構分析................................................................71
4.5.3循環伏安法分析.............................................................................72
4.5.4光學性質分析.................................................................................73
4.6綜合討論……......................................................................................77
第五章 結論與展望.........................................................................................78
5.1 結論......................................................................................................78
5.2 未來展望..............................................................................................79
參考文獻...........................................................................................................80
圖目錄
圖1.1 電致色變節能窗應用於建築體之實例...…………………………….2
圖1.2 電致色變應用…………………………………………………………4
圖2.1 典型電致色變元件基本結構示意圖…………………………………6
圖2.2 電致色變層著去色情形………………………………………………6
圖2.3 液晶電致色變顯示器…………………………………………………8
圖2.4 導電聚合物電致色變元件……………………………………………8
圖2.5 氧化鎢之單位晶胞示意圖…………………………………………..11
圖2.6 結構導向劑製作氧化鎢薄膜: (a) (b)不同比例PEG與酒精表面微
結構與(c)電致色變性質…………………………………………….16
圖2.7 氧化鋅奈米柱電極作為氧化鎢電致色變元件:(a)奈米線電極表面
微結構;(b)濺鍍氧化鎢於奈米線電極表面微結構;(c) 電致色變元
件著去色態(d)響應時間……………………………………………..17
圖2-8 氧化鋅晶體結構……………………………………………………..19
圖2-9 水熱法與其它製程之壓力溫度比較………………………………..21
圖2-10 種子層對成長氧化鋅奈米線之影響:(a) 無種子層;(b) 有種子
層…………………………………………………………………….23
圖2-11 氧化鋅奈米線成長過程…………………………………………….23
圖3.1 電沉積法實驗流程……………………………………………………25
圖3.2 氧化鋅奈米線製備流程………………………………………………26
圖3.3 調配鍍液流程…………………………………………………………27
圖3.4 電沉積法裝置示意圖…………………………………………………28
圖3-5 氧化鋅奈米線製備流程……………………………………………...29
圖3-6 試片裝置……………………………………………………………...29
圖3-7 水熱法成長設備……………………………………………………...30
圖3.7 循環伏安電位測定裝置示意圖………………………………………32
圖4.1 電沉積氧化鎢薄膜表面結構SEM圖: (a)8 (b)10 (c)12 (d) 14 mA….34
圖4.2 電沉積氧化鎢薄膜SEM側視圖: (a)8 (b)10 (c)12 (d) 14 mA……….34
圖4.3電沉積氧化鎢薄膜SEM側視圖: (a)8 (b)10 (c)12 (d) 14 mA………..36
圖4.4不同電流下沉積氧化鎢薄膜之CV圖: (a)8 (b)10 (c)12 (d) 14 mA….39
圖4.5 電沉積氧化鎢薄膜著去色光譜圖: (a)8 (b)10 (c)12 (d) 14 mA……..43
圖4.6 電沉積氧化鎢薄膜表面結構SEM圖: (a)4 (b)5 (c)6 (d)7 V………..45
圖4.7 電沉積氧化鎢薄膜SEM側視圖: (a)4 (b)5 (c)6 V…………………..45
圖4.8 電沉積氧化鎢薄膜AFM圖:(a)4 (b)5 (c)6 (d)7 V………………….47
圖4.9 不同電壓下沉積氧化鎢薄膜之CV圖: (a)4 (b)5 (c)6 V……………..49
圖4.10 電沉積氧化鎢薄膜著去色光譜圖: (a)4 (b)5 (c)6 V………………..52
圖4.11 沉積過長時間(90 s)導致薄膜龜裂之SEM圖……………………...54
圖4.12 電沉積氧化鎢薄膜表面結構SEM圖: (a)30 (b)40 (c)50 (d) 60 s…..54
圖4.13 電沉積氧化鎢薄膜SEM側視圖: (a)30 (b)40 (c)50 (d) 60 s……….55
圖4.14 電沉積氧化鎢薄膜厚度與時間比較圖……………………………..55
圖4.15 沉積不同時間氧化鎢薄膜之AFM圖:(a)30 (b)40 (c)50 (d) 60 s…57
圖4.16 沉積不同時間氧化鎢薄膜之CV圖: (a)30 (b)40 (c)50 (d) 60 s…....60
圖4.17 電沉積氧化鎢薄膜著去色光譜圖: (a)30 (b)40 (c)50(d) 60 s………63
圖4.18 電沉積氧化鎢薄膜表面結構SEM圖: (a)未退火 (b)200度(c)400
度………………………………………………………………...…..64
圖4.19 電沉積氧化鎢薄膜之AFM圖:(a)未退火 (b)200度(c)400度…..66
圖4.20 電沉積氧化鎢薄膜經退火熱處理一小時後之XRD圖:(a)400度
退火 (b)200度退火 (c)未退火……………………………………..68
圖4.21 不同溫度退火後之氧化鎢薄膜CV圖: (a)未退火 (b)200度 (c)400’
度….………………………………………………………………...70
圖4.22 不同溫度退火一小時後之氧化鎢薄膜著去色光譜圖: (a)未退火
(b)200度 (c)400度…………………………………………………72
圖4.23 水熱法成長氧化鋅奈米線5分鐘之SEM圖: (A)50k (B)100k……73
圖4.24 水熱法成長氧化鋅奈米線10分鐘之SEM圖: (A)50k (B)100k…..74
圖4.25 水熱法成長氧化鋅奈米線15分鐘之SEM圖: (a)50k (b)100k…….74
圖4.26 水熱法成長氧化鋅奈米線15分鐘之SEM側視圖…………………74
圖4.27 氧化鋅奈米線上沉積氧化鎢薄膜之SEM(a)正面圖(b)側視圖…...75
圖4.28 水熱法成長氧化鋅奈米線10分鐘之XRD圖……..………………75
圖4.29 氧化鎢薄膜沉積在不同基板上之CV圖: (a)ITO (b)AZO薄膜(c)
AZO奈米線………………………………………………………….77
圖4.30 水熱法成長不同時間摻鋁氧化鋅奈米線之穿透率光譜圖: (a)5 (b)
10 (c)15 min………………………………………………………….79
圖4.31氧化鎢薄膜沉積在不同基板上之CV圖: (a)ITO (b)AZO薄膜(c)
AZO奈米線………………………………………………………….80











表目錄
表2.1 常見過渡金屬氧化物的變色方式及性質…………………………….9
表2-2 氧化鋅物理性質特性………………………………………………...18
表2-3 氧化鋅應用範圍…………………………………………………...…19
表2-4 氧化鋅奈米線的成長方法…………………………………………...22
表3.1 化學藥品資料表………………………………………………………24
表4.1 定電流下沉積氧化鎢薄膜之各項重要參數…………………………41
表4.2 定電壓下沉積氧化鎢薄膜之各項重要參數…………………………51
表4.3 沉積不同時間下氧化鎢薄膜之各項重要參數………………………61
表4.4 電氧化鎢薄膜沉積在不同基板上之各項重要參數…………………70

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