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研究生：	陳冠中 Chen, Kuan-Chung
論文名稱：	二氧化釩粉末之製備及性質分析 Preparation and characteristics of vanadium dioxide powder
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：	2008
畢業學年度：	96
語文別：	中文
論文頁數：	69
中文關鍵詞：	水熱法、二氧化釩、熱致相變
外文關鍵詞：	Thermalchromic, vanadium dioxide, Hydrothermal
相關次數：	點閱：60 下載：8
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二氧化釩具有熱致相變之特性，其電性及光學性質能藉由改變溫度產生大幅度的變化。依此特性，VO2可作為智慧窗玻璃的塗層材料，隨著週遭環境溫度變化而自動調節紅外光進出量，藉此達到省電節能之目的。
以往對於VO2的研究都著重在VO2薄膜之製備，但其製程有著參數控制複雜、穩定性差、以及玻璃基材受到限制等之缺點。有鑒於此，本研究嘗試以水熱法一步合成VO2粉末材料，再藉由其與PMMA混合製備出VO2粉末塗料。合成粉末的特性是以XRD、SEM、DSC等儀器來分析，實驗是檢討反應助劑、水熱反應溫度及持溫時間、界面活性劑CTAB及Mo摻雜量等參數對合成VO2粉末之微觀結構及相變性質的影響。VO2粉末塗料之光學及相變性質則是藉由FTIR來量測。
由於釩的價數容易改變以及二氧化釩具多種結構，因此整個實驗過程並不僅只考慮還原反應，尚須討論由四方晶相(Tetragonal)之VO2(B)轉變為VO2(M)的過程。反應助劑的添加與否會影響反應後的生成相，而反應助劑之含量、水熱溫度及持溫時間的控制則是會對產物之晶體結構造成改變，容易形成不同結構之VO2。本研究單斜晶相(Monoclinic)之VO2(M)粉末是以V2O5粉末為原料藉由反應助劑乙醇的添加，經330℃水熱溫度持溫12小時下合成。製程中由於需經歷VO2自身之不同結構的轉換過程，而在此過程中界面活性劑CTAB會影響到反應物的生成相，導致無法達到藉由CTAB來控制產物微觀結構的效果。
在光學性質方面，VO2(M)塗料在相變為VO2(R)後能降低紅外光穿透率，而相轉換溫度為67.8℃。藉由MoO3的添加可降低VO2(M)相轉換溫度至49.0℃，但紅外光穿透變化率也隨之減少。

VO2 undergoes drastic changes in its electric and optical properties during phase transition, which adjusts the reflectance of infrared rays. For VO2, phase transition is brought about by ambient temperature changes; VO2 can therefore be used as the coating film material of intelligent windows, which results in energy savings.
Because thin films of VO2 have disadvantages such as a complex production process, instability, and restriction of glass substrate options during the preparation, in this study we therefore synthesized VO2 powder by hydrothermal method, and prepared VO2 coating by creating a mixture of VO2 and PMMA. Effects of the hydrothermal method parameters of reductant, reaction temperature, soaking time, surfactant (CTAB), and doping amount of Mo on the microstructures and phase transition properties of VO2 powder were investigated. The synthesized VO2 powder was analyzed by XRD, SEM, and EDS. The optical property of VO2 coating materials was analyzed by FTIR.
Because there are many vanadium oxide phases, and adding reductant affects these phases, our discussion includes reductant reaction and the structure transition of VO2 (M) (Monoclinic) to VO2 (R) (Tetragonal). We found that the structure of VO2 was altered by changing the reductant amounts, the hydrothermal reaction temperature and the soaking time; thus there were various structures of VO2 produced. We found that we could hydrothermally synthesize VO2 (M) powder by heating V2O5 and ethanol reductant to 330℃ for 12 hours. Our assumption that adding CTAB would help control the VO2 microstructure and allow for production of VO2 (M) was proved to be in error.
In regards to VO2’s optical properties, the transmittance of infrared rays through the VO2 coating decreased with phase transition of VO2(M)VO2(R), and phase transition temperature was 67.8℃. The phase transition temperature of VO2 powder decreased by increasing the amount of MoO3.

中文摘要......................................................................................................................Ⅰ
英文摘要......................................................................................................................Ⅱ
目錄..............................................................................................................................Ⅳ
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.......................................................................................................2
第二章	相關文獻回顧與整理...................................................................................3
  2-1 二氧化釩材料之特性與晶體結構....................................................................3
    2-1-1 二氧化釩材料之特性及其應用.................................................................3
    2-1-2 二氧化釩的晶體結構及相變化.................................................................8
  2-2 二氧化釩粉末之製備技術及其相轉變性質...................................................14
    2-2-1 二氧化釩粉末製備技術...........................................................................14
    2-2-2 摻雜物對VO2相變性質的影響...............................................................17
    2-2-3 VO2相轉變之於熱遲滯迴圈.....................................................................19
  2-3 水熱法...............................................................................................................20
    2-3-1 水熱法之原理概述...................................................................................20
    2-3-2高壓反應釜的反應容積與溫度之關係....................................................21
    2-3-3 水熱法的優點...........................................................................................22
第三章 實驗方法與步驟............................................................................................26
  3-1 實驗用起始原料...............................................................................................26
  3-2 實驗流程...........................................................................................................27
    3-2-1實驗流程圖.................................................................................................27
    3-2-2 水熱處理...................................................................................................28
    3-2-3 CTAB界面活性劑控制表面形貌.............................................................29
    3-2-4 VO2塗料的製備........................................................................................29
  3-3 粉末性質之量測..............................................................................................29
    3-3-1 結晶相鑑定...............................................................................................29
    3-3-2微觀結構觀察............................................................................................30
    3-3-3相變溫度之量測........................................................................................30
  3-4 塗料性質之量測..............................................................................................30
    3-4-1 紅外光穿透率量測..................................................................................30
第四章 結果與討論...................................................................................................33
  4-1水熱參數對釩氧化物合成之影響..................................................................33
    4-1-1反應助劑種類對釩氧化物合成相之影響...............................................33
    4-1-2乙醇添加量對釩氧化物合成相之影響...................................................41
    4-1-3 水熱溫度對釩氧化物合成相之影響......................................................43
    4-1-4 水熱持溫時間對釩氧化物合成相之影響..............................................46
    4-1-5 CTAB界面活性劑之影響........................................................................49
  4-2 摻雜 Mo 之釩氧化物粉末之製備及熱性質分析........................................52
  4-3 二氧化釩粉末塗料之光學性質分析..............................................................58
第五章 結論................................................................................................................63
參考文獻......................................................................................................................64
                                    

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