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研究生：	杜國瑞 Tu, Kuo-Juei
論文名稱：	以射頻磁控濺鍍法合成赤鐵礦薄膜與奈米銀/赤鐵礦複合薄膜之特性分析與光催化特性之研究 Study on characterization and photocatalysis of hematite thin films and nano-Ag/hematite thin films by R.F. magnetron sputtering deposition
指導教授：	陳燕華 Chen, Yen-Hua
學位類別：	碩士 Master
系所名稱：	理學院 - 地球科學系 Department of Earth Sciences
論文出版年：	2011
畢業學年度：	99
語文別：	中文
論文頁數：	76
中文關鍵詞：	赤鐵礦、薄膜、奈米銀、射頻磁控濺鍍法、可見光光催化
外文關鍵詞：	hematite, thin film, nano-Ag, R.F. magnetron sputtering deposition, photocatalysis under visible-light irradiation.
相關次數：	點閱：121 下載：5
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本研究藉由射頻磁控濺鍍法可成功地合成出赤鐵礦、奈米銀/赤鐵礦薄膜。針對赤鐵礦薄膜與奈米銀/赤鐵礦複合薄膜進行特性分析；之後把各薄膜作為光催化劑，測試薄膜在可見光下的光催化效率。在場發射掃描式電子顯微鏡（FE-SEM）的影像可發現：利用不同的濺渡時間，我們可合成出具不同晶粒大小（膜厚）的赤鐵礦薄膜；由EDS與ESCA可看到奈米金屬銀粒子確實存在複合薄膜中。從超導量子干涉振動儀的數據得知：奈米赤鐵礦薄膜的磁特性為順磁性或超順磁性，隨著膜厚增加，磁化強度也跟著變大。光催化實驗的結果證實：赤鐵礦薄膜在可見光下可有效的光催化亞甲基藍染劑，奈米銀/赤鐵礦複合薄膜因受到奈米銀粒子的影響，使得薄膜表面可反應之電子數量相對變少，造成光催化效率下降。主要原因可能為：1.因為奈米銀粒子之分佈密度太少，造成電荷轉移上之困難度，或部分的電子被捕捉困陷於中間層奈米銀粒子中。2.不能有效地分離電子電洞對。3.對可見光的吸收度下降。綜合上述結果，我們利用射頻磁控濺鍍法製備出的赤鐵礦薄膜可有效的應用在光催化有機染劑上，亦可應用於環境汙染處理上。

Hematite (Fe2O3) thin films and nano-Ag/Fe2O3 thin films can be successfully fabricated using by R.F. magnetron sputtering deposition. After preparation of the thin films, the characterization and photocatalysis under visible-light irradiation are investigated. FE-SEM images show that hematite films with different grain size (thickness) can be synthesized by adjusting the deposition time; the metallic Ag nanoparticles are really formed in the Fe2O3 matrix examined by the EDS and ESCA analyses. Moreover, The specimens exhibit paramagnetic or super-paramagnetic behavior, and the magnetization increases with the increasing film thickness. All hematite films exhibit good photocatalytic ability under visible-light illumination, and the photocatalytic activity of hematite films increases with an increase of film thickness. This is because the hematite with a thicker film thickness has a rougher surface, which provides more reaction sites for photocatalysis. However, nano-Ag/Fe2O3 films have a less photocatalysis activity than hematite films, this may be due to a decrease of electron numbers for photocatalytic reaction. The possible reasons are as follows. 1. A lower distribution density of Ag nanoparticles in the Fe2O3 films is difficult for charge transfer during photocatalytic process. 2. The electron-hole pairs can not separate effectively in the nano-Ag/Fe2O3 composites. 3. The absorbance of vis-light decreases for nano-Ag/ Fe2O3 thin films. To sum up, this study suggests that hematite thin films are superior photocatalyst under visible-light irradiation, effective for the clean removal of organic dyes, and suitable for environmental treatment applications.

目錄
 
中文摘要........................................I
英文摘要.............................................II
致謝...........................................IV
目錄.................................................V
表目錄.............................................VII
圖目錄............................................VIII
第一章 序論................................................1
1-1 前言...........................................1
1-2 研究動機與目的.............................2
第二章 文獻回顧...........................................4
2-1 赤鐵礦之特性與用途.......................4
2-2 磁控濺鍍系統之原理........................6
2-2-1 直流輝光濺鍍......................7
2-2-2 射頻濺鍍..............................9
2-2-3 磁控濺鍍..........................10
2-2-4 反應式濺鍍........................11
2-3 光催化原理....................................12
2-3-1 半導體簡介........................12
2-3-2 光催化反應........................13
2-3-3 半導體的光催化反應....................16
2-3-4 半導體光催化劑之改善...............17
2-4 光催化動力學模式..........................17
2-5銀的基本性質與光催化劑摻有奈米銀之功用...................19
第三章 研究步驟與方法...............................21
3-1 實驗流程........................................21
3-2 實驗材料........................................22
3-3 靶材製作........................................23
3-4 基板準備........................................25
3-5 赤鐵礦薄膜之製備..........................26
3-6 赤鐵礦摻有奈米銀複合薄膜之製備........................27
3-7 樣品特性分析.................................31
3-7-1 X光繞射儀.........................31
3-7-2 場發射掃描式電子顯微鏡..........................31
3-7-3 電子分析光譜儀.......................32
3-7-4固態紫可見光光譜儀..................33
3-7-5 液態紫外光/可見光光譜儀..........................33
3-7-6 超導量子干涉振動磁量儀................................34
3-7-7 原子力顯微鏡............................35
3-8 光催化特性分析.............................36
3-8-1 不照光之光催化實驗................................36
3-8-2 可見光燈下之光催化實驗...............................37
第四章 結果與討論....................................38
4-1 不同厚度之赤鐵礦薄膜特性分析..................38
4-1-1 X光繞射之結果...................38
4-1-2 場發射掃瞄式電子顯微鏡之分析結果....................41
4-1-3 超導量子干涉振動磁量儀之分析結果.......................42
4-1-4 固態紫外光/可見光光譜儀之分析結果.....................44
4-1-5 原子力顯微鏡之實驗結果................................45
4-2 光催化實驗結果............................46
4-3 奈米銀/赤鐵礦複合薄膜之特性分析.....................49
4-3-1 X光繞射之結果..................49
4-3-2 場發射掃瞄式電子顯微鏡之分析結果......................51
4-3-3 超導量子干涉震動磁量儀之分析結果......................53
4-3-4 電子分析光譜儀之分析結果..............................54
4-3-5 固態紫外光/可見光光譜儀之分析結果..................55
4-3-6 原子力顯微鏡之實驗結果.............................55
4-4奈米銀/赤鐵礦複合薄膜之光催化結果..........................57
4-5 與前人文獻之比較..................................60
第五章結論................................................63
5-1 不同厚度赤鐵礦薄膜之光催化能力比較...................63
5-2 奈米銀/赤鐵礦複合薄膜之光催化能力比較....................63
5-3 單層赤鐵礦與複合薄膜之光催化能力比較................63
參考文獻.........................................65

 
表目錄
 

表 2-1 赤鐵礦的基本性質...........................................................................................5
表 2-2 銀的基本性質.................................................................................................20
表 3-1 赤鐵礦薄膜之製程參數.................................................................................29
表 3-2 單層赤鐵礦薄膜摻有奈米銀粒子之製程參數.............................................30
表 4-1 薄膜樣品代號對照表.....................................................................................38
表 4-2 單層赤鐵礦粒徑大小計算值.........................................................................41
表 4-3單層赤鐵礦XRD繞射峰強度與標準樣品比值............................................41
表 4-4 單層赤鐵礦光催化之實驗相關數據.............................................................49
表 4-5 複合薄膜粒徑大小計算值.............................................................................50
表 4-6複合薄膜樣品XRD繞射峰強度與標準樣品比值.........................................51
表 4-7 複合薄膜之光催化實驗數據.........................................................................60
表 4-8 赤鐵礦薄膜光催化性質之比較.....................................................................62

 
圖目錄

 
圖2-1 赤鐵礦的晶體結構示意圖................................................................................5
圖2-2 鐵氧化物的相圖................................................................................................6
圖2-3 濺鍍原理之示意圖............................................................................................7
圖2-4 直流輝光放電之示意圖....................................................................................8
圖2-5 陰極與陽極電位分布之示意圖........................................................................9
圖2-6射頻磁控濺鍍法之示意圖................................................................................10
圖2-7 磁控濺鍍法之示意圖......................................................................................11
圖2-8 反應式濺鍍法之示意圖..................................................................................12
圖2-9 導體、半導體與絕緣體之差異示意圖..........................................................13
圖2-10 光催化反應示意圖........................................................................................14
圖3-1 實驗流程圖......................................................................................................22
圖3-2 赤鐵礦靶材之燒結流程..................................................................................25
圖3-3複合薄膜製程示意圖.......................................................................................28
圖3-4亞甲基藍之檢量線...........................................................................................34
圖3-5 不照光下光催化實驗示意圖..........................................................................36
圖3-5 不照光之光催化實驗示意圖..........................................................................37
圖4-1 不同濺鍍時間之赤鐵礦薄膜的X光繞射圖譜..............................................40
圖4-2 單層赤鐵礦薄膜之SEM影像.........................................................................43
圖4-3 不同濺鍍時間下單層赤鐵礦薄膜的磁特徵曲線..........................................44
圖4-4 不同濺鍍時間下單層赤鐵礦薄膜對可見光的吸收度與能隙圖..................45
圖4-5 單層赤鐵礦薄膜之原子力顯微鏡影像..........................................................46
圖4-6 不同濺鍍時間之單層赤鐵礦薄膜的可見光光催化亞甲基藍之濃度降解圖......................................................................................................................48
圖4-7 不同濺鍍時間之單層赤鐵礦薄膜的可見光光催化亞甲基藍L-H模式分析圖.....................................................................................................................48
圖4-8 複合薄膜之X光繞射圖譜.............................................................................50
圖4-9 複合薄膜之表面形貌......................................................................................52
圖4-10 2H/Ag/2H複合薄膜的表面形貌....................................................................52
圖4-11 樣品Ag/4H之能量散佈光譜儀之分析圖譜................................................53
圖4-12 複合膜之磁特性曲線圖................................................................................54
圖4-13 銀的3d5/2與3d3/2的X光能譜分析圖..........................................................54
圖4-14 複合薄膜對可見光的吸收度與能隙圖........................................................55
圖4-15 複合薄膜之原子力顯微鏡影像....................................................................56
圖4-16 奈米銀/赤鐵礦複合薄膜的可見光光催化效率圖.......................................59
圖4-17 複合薄膜的可見光光催化之L-H模式分析圖..........................................59
圖4-18赤鐵礦單層膜與複合膜之光催化效果比較圖...........................................60

                                    

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