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研究生:張哲揚
研究生(外文):Che-Yang Chang
論文名稱:以射頻濺鍍法及液相沉積法成長電致變色氧化鎢薄膜
論文名稱(外文):Electrochromic Properties of Tungsten Oxide Films Prepared by RF Sputtering and Liquid Phase Deposition
指導教授:李明逵
指導教授(外文):Ming-Kwei Lee
學位類別:碩士
校院名稱:國立中山大學
系所名稱:電機工程學系研究所
學門:工程學門
學類:電資工程學類
論文種類:學術論文
論文出版年:2009
畢業學年度:97
語文別:英文
論文頁數:99
中文關鍵詞:射頻濺鍍法氧化鎢液相沉積法電致變色
外文關鍵詞:RF sputteringLPDWO3electrochromic
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對於各種各樣的光元件特別在電致變色領域上三氧化鎢薄膜是重要的材料。以射
頻濺鍍法沈積氧化鎢薄膜在導電玻璃底層(銦錫氧化物/玻璃)上,射頻功率100
瓦,透過氧化鎢陶瓷靶材,在10毫托的總氣壓下,氧和氬流量比率(0比1)沉積薄
膜。我們利用不同的氣體環境退火後增進氧化鎢薄膜電致變色的特性。
此外,混合氫氟酸和硝酸並溶解鎢金屬屬粉末, 將其用去離子水稀釋備製成長
溶液(氫氟酸鎢)加入濃度0.1莫耳的硼酸或鋁,在攝氏40度的環境下以液相沉積
法成長氧化鎢薄膜。
在我們的實驗過程中,以掃描電子顯微鏡觀察薄膜表面型態,以X光繞射分析其
結構,化學性能以X光電子能譜以及傅裡葉轉換紅外線光譜分析化學特性,以
spectrophotometer(MP-100 M)分析光學性能,以及以循環伏安儀觀察薄膜的電
致變色特性 .
在我們實驗結果中,我們發現以射頻濺鍍製成的氧化鎢薄膜在氧氣環境退火後的
光學與電致變色特性。另外也嘗試以液相沉積法藉由氟化物溶液在(銦錫氧化物/
玻璃)基板上沉積氧化鎢薄膜。
Tungsten trioxide (WO3) films are important for various optical devices and
especially for electrochromic materials. Sputtered WO3 thin films were deposited on
conductive glass substrate (ITO/glass) by RF sputtering from a WO3 target(diameter
2”x 6 mm) in a reactive atmosphere of oxygen and argon flow ratio(0 to 1) mixture in
a total gas pressure of 10m Torr. The RF power was 100W operating at 13.56MHz.We
will improve the WO3 films by post-annealing in different atmosphere ambient.
In addition, to prepare treatment solution of growing WO3 films were dissolved
tungsten to aqueous which mixed hydrofluoric acid and nitric acid until it
supersaturate. This solution was then diluted to 0.02 M of tungsten ions with distilled
water. And we can get the treatment solution (WO3-HF aqueous). The WO3 thin films
have been deposited at 40oC with the treatment solution (WO3-HF aqueous) which
full of W ions, the 0.1M boric acid (H3BO3) solution and added aluminium metal by
liquid phase deposition (LPD) technique. The deposition rate could be controlled to
45 nm/h.
In our experiment, the WO3 films morphology and thickness was characterized
by scanning electron microscopy(SEM), structure was characterized by X-ray
diffraction(XRD), chemical properties was characterized by X-ray photoelectron
spectroscopy(XPS) and Fourier transform infrared spectroscopy(FT-IR), optical
properties was characterized by spectrophotometer(MP-100M), and electrochromic
characterized by cyclic voltammetry(CHI627C).
In our results, it will be improved the optical and electrochromic properties of
sputtered-WO3 films by post-annealing in O2 ambient. we also have try a novel and
very simple process for the thin films of WO3 by the LPD process. Adherent and
conformal WO3 electrochromic films were prepared on ITO/glass from aqueous
fluoride solution.
CHAPTER 1 …………………………………………………………………………1
INTRODUCTION........................................................................................................1
1-1 Background of Electrochromic.....................................................................1
1-2 Applications of Electrochromic Device........................................................3
1-3 Tungsten trioxide ...........................................................................................4
1-4 Motivation of RF sputtering .........................................................................4
1-5 Advantage of RF sputtering..........................................................................4
1-6 Motivation of LPD.........................................................................................5
1-7 Mechanisms of LPD.......................................................................................5
1-8 Advantage of LPD .........................................................................................6
REFERENCES.............................................................................................................9
CHAPTER 2...............................................................................................................10
EXPERIMENTS ........................................................................................................10
2-1 Preparation of Substrate.............................................................................10
2-1.1 ITO-coated glass Cleaning Procedures...........................................10
2-1.2 Photoresist coated(Lithography).....................................................10
2-2 PART I: Prepared by RF Sputtering.........................................................11
2-2-1 View of RF Sputtering Technique ...................................................11
2-2-2 The Process of Sputter-WO3 Films.................................................12
2-2-3 Thermal Treatment of WO3 Films by RF Sputtering ...................13
2-3 PART II: Prepared by Liquid Phase Deposition.......................................13
2-3-1 Liquid Phase Deposition System.....................................................13
2-3-2 Preparation of Deposition Solutions...............................................14
(a) Preparation of WO3-HFaq Solution.............................................14
(b) Preparation of H3BO3 Solution...................................................14
2-3-3 Deposition of LPD-WO3 Films ........................................................15
2-4 Characteristics of WO3 Films.....................................................................15
2-4-1 Physical Property .............................................................................15
(a) SEM (scanning electron microscopic)...........................................15
(b) XRD (X-ray diffraction) ................................................................15
2-4-2 Chemical Property ...........................................................................16
(a) XPS (X-ray photoelectron spectroscopy) ......................................16
(b) FTIR (Fourier transform infrared spectroscopy)...........................16
2-4-3 Optical Property (Spectrophotometer) ..........................................16
2-4-4 Electrochemical Property (Cyclic voltammetry)...........................16
CHAPTER 3...............................................................................................................24
IV
RESULTS AND DISCUSSION ................................................................................24
3-1 Electrochromic Reaction.............................................................................24
3-2 PART I: Characteristics of Sputtered-WO3 Films....................................26
3-2-1 Physical Properties of Sputtered-WO3 Films ................................26
3-2-1.1 Deposition of Sputtered-WO3 Film......................................26
3-2-1.2 SEM view of Sputtered- WO3 Film .....................................26
3-2-1.3 XRD Patterns of Sputtered-WO3 Films ..............................27
3-2-2 Optical Properties of The Sputtered-WO3 Films ..........................28
3-2-3 Chemical Properties of The Sputtered-WO3 Films.......................29
3-2-3.1 XPS Analysis of The Sputtered-WO3 Films ........................29
3-3-3.2 FTIR Spectra of The Sputtered-WO3 Films .......................30
3-2-4 Electrochemical Property of The Sputtered-WO3 Films..............30
3-3 PART II: Characteristics of LPD-WO3 Films ...........................................32
3-3-1 Physical Properties of The LPD-WO3 Films..................................32
3-3-1.1 Deposition of LPD- WO3 Film .............................................32
3-3-1.2 SEM view of LPD-WO3 Film ...............................................32
3-3-1.3 XRD Patterns of LPD- WO3 Films ......................................32
3-3-2 Optical Properties of The LPD- WO3 Films ..................................33
3-3-3 Chemical Properties of The LPD-WO3 Films................................33
3-3-3.1 XPS Analysis of The LPD-WO3 Films.................................33
3-3-4 Electrochemical Property of LPD-WO3 Films ..............................34
REFERENCES...........................................................................................................81
CHAPTER4................................................................................................................83
CONCLUSIONS........................................................................................................83
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