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研究生：	李卓翰 Lee, Cho-Han
論文名稱：	二氧化釩薄膜之製備及其性質研究 Preparation and characteristics of vanadium dioxide thin film
指導教授：	黃啟祥 Hwang, Chii-Shyang
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：	2006
畢業學年度：	94
語文別：	中文
論文頁數：	86
中文關鍵詞：	二氧化釩薄膜、無機溶膠凝膠法
外文關鍵詞：	VO2 thin film, Inorganic sol gel method
相關次數：	點閱：251 下載：5
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VO2具有溫度相變的特性，特別是電性及光學等性質會隨相變而發生急遽之變化。VO2可作為智慧窗玻璃的塗層薄膜材料，可隨週遭溫度變化而調節紅外線反射率，具有節約能源之功用。
以往VO2薄膜的製備是需在具有危險性的CO還原氣氛下操作。為改善此缺點，本研究針對其製程加以改進，研究方法包括以無機溶膠凝膠法製備V2O5溶膠，並將之浸鍍於石英玻璃基板上，再藉由碳粉將V2O5膜還原為VO2薄膜。實驗是藉由TG/DTA、Viscometer等儀器來分析V2O5溶膠的特性；利用XRD、SEM、FTIR、Four-probe等儀器來分析VO2薄膜的特性；並檢討乾燥條件、煅燒溫度、持溫時間、浸鍍次數及Mo之摻雜量對VO2薄膜微觀結構及相變性質之影響。
製備的V2O5膜於N2下經550℃以上煅燒後即可形成VO2(M)薄膜，VO2之結晶性是隨煅燒溫度之增加而增加。VO2薄膜之表面是由圓形顆粒和空隙所組成，其顆粒大小是隨著煅燒溫度及持溫時間之增加而增大，隨著浸鍍次數之增加，薄膜表面之粗糙度也隨之增大。
在光學及電性質方面，隨著煅燒溫度及持溫時間之增加，VO2(M)薄膜之紅外光穿透率會隨之上升，而其熱滯迴圈寬度與相轉變溫度則會隨之減小(69.5℃68℃)。隨著浸鍍次數(薄膜厚度)之增加，紅外光穿透變化率會隨之增加，而熱滯迴圈寬度與相轉變溫度並無明顯變化。
隨著Mo摻雜量之增加，VO2薄膜之電阻及紅外光穿透率隨之減少，相轉變溫度亦會隨之降低。甚至低至35℃。

VO2 has a property of phase transition. When VO2 undergoes phase transition, accompanied by drastic changes in electric and optical properties. VO2 can adjust reflectance of infrared rays when ambient temperature changes. Therefore, it can be as the coatings film material of intelligent window with saving energy effect.
In order to improve the need of operating in dangerous CO reduction atmosphere during preparing VO2 thin film in the past. We improved the process in this study. The method included applying inorganic sol-gel method to prepare V2O5 sol then V2O5 film was forming on fused silica after dipped into the sol. Then, we used carbon powder to reduce V2O5 to VO2 thin film. The preparing V2O5 sol was characterized by TG/DTA、Viscometer；the synthesized VO2 thin film was analyzed by XRD、 SEM、FTIR、Four-probe. Effects of parameters of drying conditions、calcination temperature、 holding time 、 dipping times and doping amount of Mo on microstructure and phase transition properties of VO2 film were investigated.
VO2 (M) thin film was formed by calcining V2O5 film at 550℃ in N2, and the crystallization increased with temperature. The surface of VO2 thin film was composed of round shape particles and voids, and the size of particle increased with calcinations temperature and holding time increased. The roughness of film surface increased with dipping times increased.
In optical and electrical properties, the transmittance of infrared ray of VO2 (M) thin film increased and the heat hysteretic width and phase transition temperature decreased (69.5℃68℃) with calcinations temperature and holding time increased. the transmittance of infrared ray and the heat hysteretic width and phase transition temperature increased with dipping times (film thickness) increased.
The electric resistance and infrared ray of VO2 thin film decreased with adding amount of Mo increased. The phase transition temperature also even lowered to 35℃.

中文摘要..............................................................Ⅰ
英文摘要...........................................Ⅱ
目錄.............................................................................................................................Ⅲ
表目錄……………...…………...................................................................................Ⅵ
圖目錄.........................................................................................................................Ⅶ
第一章 緒論..................................................................................................................1
1-1前言......................................................................................................................1
1-2 研究目的.............................................................................................................1
第二章 相關文獻回顧與整理......................................................................................2
2-1 二氧化釩之性質與晶體結構.............................................................................2
2-1-1 二氧化釩之特性及其應用........................................................................2
2-1-2 二氧化釩的晶體結構................................................................................5
2-2 二氧化釩薄膜之製備技術及其相轉變性質.....................................................8
2-2-1 二氧化釩薄膜製備技術.............................................................................8
2-2-2 無機V2O5溶膠之製備...................................................................................11
2-2-3 VO2相轉變之熱遲滯迴圈........................................................................12
2-2-4 摻雜不純物對相變溫度的影響..............................................................13
2-2-5 摻雜不純物對薄膜電性的影響..............................................................16
2-2-6 摻雜不純物對薄膜光學性能的影響......................................................18
2-3 溶膠凝膠法之原理概述.................................................................................20
2-3-1 溶膠凝膠法之製備技術..........................................................................22
2-3-2 溶膠凝膠法之應用與優點......................................................................25
2-4 浸鍍塗佈法之原理.........................................................................................26
第三章 實驗方法與步驟............................................................................................28
3-1 實驗用起始原料及基板.................................................................................28
3-2 實驗流程.........................................................................................................29
3-2-1 實驗流程圖.............................................................................................29
3-2-2 溶膠的配製.............................................................................................30
3-2-3 基板的處理.............................................................................................30
3-2-4 薄膜成長及熱處理條件..........................................................................30
3-3 溶膠性質之量測.............................................................................................31
3-3-1黏度量測...................................................................................................31
3-3-2 熱差/質差分析.........................................................................................31
3-4 薄膜性質之量測.............................................................................................31
3-4-1 薄膜厚度量測..........................................................................................31
3-4-2 結晶相鑑定..............................................................................................32
3-4-3 微觀結構觀察..........................................................................................32
3-4-4 化學鍵結分析..........................................................................................32
3-4-5 紅外光穿透率量測..................................................................................33
3-4-6 電性質量測..............................................................................................33
3-4-7 可見光透光度量測..................................................................................34
第四章 結果與討論....................................................................................................37
4-1 V2O5溶膠之性質..............................................................................................37
4-1-1 靜置時間對溶膠黏度之影響..................................................................37
4-1-2 凝膠的熱差-質差分析.............................................................................38
4-2 VO2薄膜之製備...............................................................................................40
4-2-1 乾燥條件對薄膜起泡現象之影響..........................................................40
4-2-2 薄膜厚度的成長......................................................................................43
4-3 釩氧化物薄膜性質分析.................................................................................46
4-3-1 合成薄膜之結晶相鑑定..........................................................................46
4-3-2 合成薄膜之微觀結構分析......................................................................49
4-3-3合成薄膜之化學鍵結分析.......................................................................56
4-3-4 合成薄膜之紅外光譜分析......................................................................58
4-3-5 合成薄膜之電性質分析..........................................................................69
4-3-6 合成薄膜之可見光穿透率分析..............................................................70
4-4 摻雜Mo之釩氧化物薄膜性質分析..............................................................77
4-4-1合成薄膜之微觀結構分析.......................................................................77
4-4-2合成薄膜之紅外光譜分析.......................................................................77
4-4-3合成薄膜之電性質分析...........................................................................78
第五章 結論........................................................................................................................82
參考文獻..............................................................................................................................83

                                    

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