以溶凝膠法製作摻錫氧化鐵薄膜並研究其在光電分解水之應用

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研究生：	簡戩 Chien Chien
論文名稱：	以溶凝膠法製作摻錫氧化鐵薄膜並研究其在光電分解水之應用 On the fabrication of Sn-doped Fe2O3 thin films by sol-gel process and their application to photoelectrochemical water splitting
指導教授：	林景崎
口試委員:
學位類別：	碩士 Master
系所名稱：	工學院 - 機械工程學系 Department of Mechanical Engineering
論文出版年：	2015
畢業學年度：	103
語文別：	中文
論文頁數：	98
中文關鍵詞：	光電化學法、溶膠凝膠法、氧化鐵薄膜、錫摻雜、二次退火
相關次數：	點閱：14 下載：0
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本論文於披覆摻氟氧化錫(F-doped SnO2, FTO)玻璃基板上，以溶凝膠法搭配旋轉塗佈製程成長氧化鐵薄膜，並探討其應用於光電化學分解水產氫之功能。研究內容在於改變前驅物中螯合劑(polyvinylpyrrolidone, PVP)之濃度、旋轉塗佈層數製作多層氧化鐵薄膜，進而施以二次熱處理研究錫自FTO擴散至氧化鐵薄膜之情形，探討此多層膜氧化鐵之晶體結構、光學性質和光電化學特性。結果顯示: 上述製程所得之多層氧化鐵薄膜，經掃描式電子顯微鏡(SEM)觀察到具有多孔表面之結構；經X光繞射分析(XRD)及拉曼(Raman)光譜分析得知: 此多層氧化鐵薄膜經550 ℃退火2小時後，皆呈現為多晶赤鐵礦(α-Fe2O3, hematite)且未出現二次相；經偏壓0.6 V (vs. SCE)光電化學測試結果顯示: 當螯合劑濃度與鐵之比例為2 (PVP/Fe = 2) ，且經旋轉塗佈8層之薄膜試片較其他層數薄膜具有較高之光電流(0.015 mA/cm2)。若此經550 ℃退火之8層薄膜再經750℃二次退火之試片，偵測其光電流，發現增高至0.03 mA/cm2，究其原因:係由錫離子自FTO基板擴散至氧化鐵薄膜中，提高其載子濃度所致。
為了解錫離子之作用，故意製作錫摻雜自氧化鐵薄膜。製程如同上述，僅在前驅溶液中添加含二價及四價之氯化錫溶液來造成薄膜摻雜。在2.5、5、7.5及10 at.% 四種摻錫氧化鐵薄膜中，經550 ℃退火2小時後，含7.5 at.%之錫摻雜薄膜測得最佳之光電流密度(0.023 mA/cm2 bias 0.6 V vs. SCE)；以X光光電子能譜儀(XPS)分析可得知:無論摻雜二價或四價錫離子，薄膜在經過退火後均已轉變成四價錫離子之摻雜。

In this study, the sol-gel and spin coating methods are used to fabricate α-Fe2O3-based thin films on fluorine-doped SnO2 (FTO) glass substrates which is used as a photoelectrode for photoelectrochemical (PEC) water splitting. In the first part, effects of polyvinylpyrrolidone (PVP) concentrations and spin-coating times on the microstructural, morphological, optical and electrochemical and PEC properties of pure α-Fe2O3 thin films are investigated. In the second part, we attempted to prepare Sn-doped α-Fe2O3 thin films for PEC water splitting via two types of impurity-doping (i.e., re-annealed at higher temperature or directly added tin chloride to our precursor solutions). The results from scanning electron microscope showed that the pure α-Fe2O3 thin films revealed a porous films on the surface of sample. After annealing at 550 oC in air ambient, all samples belonged polycrystalline hematite structure and no secondary phase via X-ray diffraction patterns and Raman spectra. From PEC performance, the sample deposited via PVP/Fe concentration ratio of 2 and spin-coating times of 8 times which has a higher photocurrent of 0.015 mA/cm2 than other samples. In the section of Sn-doping, we found that the specimen with re-annealing at 750 oC has a better PEC response due to the high temperature of re-annealing allowed the tin ion diffused from the substrate into iron oxide crystalline which increased the carrier concentration leading a higher PEC performance. On the other hand, we found that the 7.5% Sn-doped α-Fe2O3 thin films has a higher PEC response than other samples which prepared via directly added tin chloride to our precursor solutions. It is noticed that no matter whether added divalent or tetravalent tin ion, after annealing, they all became tetravalent tin ion and bonding with iron which were analyzed by X-ray photoelectron spectroscopy.

目錄
中文摘要……………………………………………………………….v
Abstract………………………………………………………………vii
致謝………………………………………………………………….viii
目錄……………………………………………………………………ix
表目錄……………………………………………………………….xiii
圖目錄……………………………………………………………… xiv

第一章、 緒論    1
1-1 前言    1
1-2 研究動機    2
1-3 研究目的    4
第二章、研究理論與文獻回顧    5
2-1 半導體    5
2-2 光觸媒    6
2-3 光電化學水分解    8
2-4 影響光催化之因素    9
2-5 氧化鐵光觸媒    11
2-6 溶膠凝膠    13
2-7 文獻整理    15
第三章、 實驗方法與步驟    18
3-1 實驗規劃    18
3-2 實驗藥品    18
3-3 實驗儀器設備    19
3-3-1 實驗設備    19
3-3-2 分析儀器    20
3-4 實驗流程    21
3-5 光陽極製備    21
3-5-1 基材前處理    21
3-5-2 前驅物調配    22
3-5-3 旋轉塗佈    22
3-5-4 熱處理    23
3-5-5 電極封裝    24
3-6 材料分析    24
3-6-1 X-ray 繞射儀    25
3-6-2 場發射掃描式電子顯微鏡    26
3-6-3 拉曼光譜分析儀    26
3-6-4 X 射線光電子能譜儀(X-ray photoelectron spectroscopy, XPS)    27
3-6-5 紫外-可見光光譜儀 (UV -Visible Spectrophotometer)    27
3-6-6 恆電位儀    28
第四章、 實驗結果    30
4-1氧化鐵薄膜    31
4-1-1 螯和劑濃度對氧化鐵的影響    31
4-1-2 膜厚對氧化鐵的影響    34
4-2 非蓄意掺雜錫對氧化鐵的影響(高溫二次退火)    37
4-2-1 表面形貌與粒徑大小的觀察    38
4-2-2 晶體結構分析    38
4-2-3 紫外光-可見光光譜分析    39
4-2-4 光電化學量測    39
4-3 蓄意掺雜錫對氧化鐵的影響    41
4-3-1 四價錫的摻雜    41
4-3-2 二價錫的摻雜    44
第五章、 討論    47
5-1氧化鐵薄膜    47
5-1-1 螯和劑濃度對氧化鐵的影響    47
5-1-2 膜厚對氧化鐵的影響    49
5-2 非蓄意掺雜錫對氧化鐵的影響(高溫二次退火)    50
5-3蓄意掺雜錫對氧化鐵的影響    53
5-3-1 四價錫的摻雜    53
5-3-2 二價錫的摻雜    54
第六章、 結論    56
第七章、 未來展望    58
參考文獻    59
























表目錄
表3- 1實驗藥品    65


































圖目錄
圖1- 1本多-藤島效應實驗示意圖    66
圖1- 2太陽光能量分佈示意圖    66
圖1- 3 α-Fe2O3可見光光觸媒可利用之太陽光波長    67
圖2- 1 (a)絕緣體，(b)半導體及(c)導體的能帶圖示    68
圖2- 2光觸媒在物理和化學方面的應用    69
圖2- 3光電化學反應示意圖    69
圖2- 4 光觸媒半導體的能帶間隙    70
圖3- 1超音波震盪器    70
圖3- 2箱型燒結爐    71
圖3- 3旋轉塗佈機    71
圖3- 4實驗流程圖    72
圖3- 5 旋轉塗佈之轉速對時間之關係圖    73
圖3- 6 熱處理昇溫參數    73
圖3- 7光電化學量測系統    74
圖4- 1 不同螯合劑濃度的氧化鐵薄膜之SEM,(a)~(c)分別為PVP/Fe=1.5, PVP/Fe=2, PVP/Fe=2.5在5萬倍率下之圖形    74
圖4- 2 不同螯合劑濃度濃度的氧化鐵薄膜之XRD    75
圖4- 3 不同螯合劑濃度的氧化鐵薄膜之Raman    75
圖4- 4不同螯合劑濃度濃度的氧化鐵薄膜的吸收光譜    76
 圖4- 5 不同螯合劑濃度濃度的氧化鐵薄膜的光穿透率    76
圖4- 6不同螯合劑濃度濃度的氧化鐵薄膜的光學能隙    77
圖4- 7 不同螯合劑濃度濃度的氧化鐵薄膜的光電流密度    77
圖4- 8 不同螯合劑濃度濃度的氧化鐵薄膜的交流阻抗    78
圖4- 9塗佈不同層數的氧化鐵薄膜之SEM,(a)~(d)分別為6,8,10,12層在3萬倍率之下的圖形    78
圖4- 10不同塗佈層數的氧化鐵薄膜之橫截面SEM,(a)~(f)分別為4,6,8,10,12層在3萬倍率之下的橫截面圖形    79
圖4- 11不同塗佈層數的氧化鐵薄膜之XRD    79
圖4- 12不同塗佈層數的氧化鐵薄膜之Raman    80
圖4- 13不同塗佈層數的氧化鐵薄膜的吸收光譜    80
圖4- 14不同塗佈層數的氧化鐵薄膜的穿透率    81
圖4- 15不同塗佈層數的氧化鐵薄膜的光學能隙    81
圖4- 16不同塗佈層數的氧化鐵薄膜的光電化學分析    82
圖4- 17不同二次退火溫度的氧化鐵薄膜之SEM    82
圖4- 18不同二次退火溫度的氧化鐵薄膜之XRD    83
圖4- 19 不同二次退火溫度的氧化鐵薄膜之Raman    83
圖4- 20不同二次退火溫度的氧化鐵薄膜之吸收光譜    84
圖4- 21不同二次退火溫度的氧化鐵薄膜之光穿透率    84
圖4- 22不同二次退火溫度的氧化鐵薄膜之光學能隙    85
圖4- 23不同二次退火溫度的氧化鐵薄膜之PEC    85
圖4- 24不同二次退火溫度的氧化鐵薄膜之XPS    86
圖4- 25不同二次退火溫度的氧化鐵薄膜之Mott-Schottky(M-S)分析結果    86
圖4- 26不同二次退火溫度的氧化鐵薄膜之TEM    87
圖4- 27不同二次退火溫度的氧化鐵薄膜之TEM    88
圖4- 28不同四價錫摻雜濃度的氧化鐵薄膜之SEM    88
圖4- 29不同四價錫摻雜濃度的氧化鐵薄膜之XRD    89
圖4- 30不同四價錫摻雜濃度的氧化鐵薄膜之Raman    89
圖4- 32不同四價錫摻雜濃度的氧化鐵薄膜之光穿透率    90
圖4- 33不同四價錫摻雜濃度的氧化鐵薄膜之光學能隙    91
圖4- 34不同四價錫摻雜濃度的氧化鐵薄膜之PEC    91
圖4- 35不同四價錫摻雜濃度的氧化鐵薄膜之Mott-Schottky(M-S)分析    92
圖4- 36不同四價錫摻雜濃度的氧化鐵薄膜之EIS    92
圖4- 37不同四價錫摻雜濃度的氧化鐵薄膜之TEM    93
圖4- 38不同四價錫摻雜濃度的氧化鐵薄膜之TEM    94
圖4- 39不同二價錫摻雜濃度的氧化鐵薄膜之SEM    94
圖4- 44不同二價錫摻雜濃度的氧化鐵薄膜之PEC    97
圖4- 45不同二價錫摻雜濃度的氧化鐵薄膜之EIS    97
圖4- 46不同二價錫摻雜濃度的氧化鐵薄膜之XPS    98



                                

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