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研究生:羅士傑
研究生(外文):Shih-Chieh Lo
論文名稱:利用脈衝雷射成長奈米結構之氧化鐵薄膜應用於光電化學產氫
論文名稱(外文):Growth of hematite nanostructure film for photoelectrochemial hydrogen production by pulsed laser deposition
指導教授:曾重仁
指導教授(外文):Chung-Jen Tseng
學位類別:碩士
校院名稱:國立中央大學
系所名稱:能源工程研究所
學門:工程學門
學類:綜合工程學類
論文種類:學術論文
論文出版年:2015
畢業學年度:103
語文別:中文
論文頁數:82
中文關鍵詞:脈衝雷射沉積法光電化學產氫奈米結構氧化鐵
外文關鍵詞:Pulsed laser depositionPhotoelectrochemical hydrogen productionnanostructureHematiteα-Fe2O3
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本研究利用脈衝雷射濺鍍沉積(Pulsed-laser deposition method, PLD)製備
氧化鐵奈米柱陣列薄膜於FTO 導電玻璃上,再利用熱處理法以進行晶體結
構之強化,並探討以脈衝雷射濺鍍沉積製備氧化鐵機制以及熱處理各項參
數的改變對氧化鐵薄膜物理特性及光電化學性質的影響。
以X-ray 繞射分析儀檢測,氧化鐵薄膜經由PLD 與熱處理之晶體結構
變化,發現PLD 之雷射通量100 J/cm2 有優選[110]。以掃描式電子顯微鏡觀
察沉積之奈米柱結構的表面型態及側面的柱狀結構,則PLD 之氧壓16
Pa~29 Pa 有奈米柱陣列的產生。以紫外光/可見光/近紅外光光譜儀檢測不同
奈米柱陣列對光吸收性之影響,則奈米柱內部之氧化鐵顆粒由圓形到長條
形的階段,光吸收率會逐漸上升。在光電化學量測上,以1 M 的KOH 水溶
液為電解液,由Mott-Schottky 分析得知隨著熱處理之氧壓下降,其載子濃
度越高,有利於電化學反應的產生;以AM 1.5 太陽光模擬器,氧化鐵薄膜
相對於參考電極Ag/AgCl 之偏壓0 V 時,最佳的光電流密度值為0.13
mA/cm2。
Pulsed laser deposition (PLD) was used to prepare α-Fe2O3 nanorod array
thin film on FTO glass, followed by annealing to improve crystal structure.
Effects of PLD parameters and annealing parameters on the physical properties
and photoelectrochemical properties of α-Fe2O3 film are also investigated.
By comparing crystal structures using XRD analysis for different PLD and
annealing parameters, we found PLD fluence of 100 J/cm2 resulted in crystals
with [110] preference. Using SEM to observe the surface and cross-sectional
morphology of α-Fe2O3 nanorod, we found PLD oxygen pressure of 16 Pa to 29
Pa successfully grow nanorod array thin film. In addition, we found that the
absorption coefficient increases when the gran shape of α-Fe2O3 changes from
spherical to ellipsoidal. From Mott-Schottky analysis, carrier density is found to
increase as the oxygen pressure in annealing process decreases. Under AM 1.5
solar irradiation, the photocurrent density is found to be 0.13 mA/cm2 with zero
applied potential vs. Ag/AgCl.
中文摘要…………………………………………………………………………I
Abstract…………………………………………………………………………II
目錄…………………………………………………………………………….III
圖目錄…………………………………………………………………………VII
表目錄…………………………………………………………………………..X
第一章、 緒論…………………………………………………………………..1
1.1. 研究背景………………………………………………………………….1
1.2. 研究動機………………………………………………………………….2
第二章、 文獻回顧……………………………………………………………..4
2.1. 光電化學水分解…………………………………………………………...4
2.2. 半導體光觸媒……………………………………………………………...5
2.2.1. 半導體能帶理論…………………………………………………………6
2.2.2. 半導體水溶液介面性質…………………………………………………8
2.2.3. 目前常見的半導體光觸媒材料………………………………………..11
2.3. 氧化鐵光觸媒…………………………………………………………….12
2.4. 奈米材料………………………………………………………………….15
2.4.1. 奈米材料之維度………………………………………………………..15
2.4.2. 奈米材料之特性………………………………………………………..16
2.4.3. 奈米材料之應用………………………………………………………..18
2.5. 脈衝雷射濺鍍沉積法…………………………………………………….18
2.6. 熱處理…………………………………………………………………….19
2.7. 研究目的………………………………………………………………….20
第三章、 實驗方法……………………………………………………………21
3.1. 靶材、基材、氣體及實驗藥品………………………………………….21
3.1.1. 靶材準備………………………………………………………………..21
3.1.2. 基材準備………………………………………………………………..21
3.1.3. 奈米結構薄膜製備……………………………………………………..21
3.1.4. 分析準備………………………………………………………………..21
3.2. 儀器設備………………………………………………………………….22
3.2.1. 靶材製備………………………………………………………………..22
3.2.2. 基材準備………………………………………………………………..22
3.2.3. 奈米結構薄膜製備……………………………………………………..22
3.2.4. 分析儀器………………………………………………………………..22
3.3. 實驗流程………………………………………………………………….23
3.3.1. 靶材製備………………………………………………………………..23
3.3.2. 基材準備………………………………………………………………..24
3.3.3. 脈衝雷射濺鍍沉積氧化鐵奈米結構薄膜……………………………..25
3.3.4. 熱處理…………………………………………………………………..27
3.3.5. 電極封裝……………………………………………………………..…27
3.4. 奈米結構薄膜之特性分析...……………………………………………..28
3.4.1. X-ray 繞射分析儀………………………………………………….........29
3.4.2. 紫外光-可見光-近紅外光光譜儀……………………………...………29
3.4.3. 場發射式電子顯微鏡…………………………………………..……....29
3.4.4. 恆電位儀………………………………………………………..….…...30
3.4.4.1. 光電流密度…………………………………………………..…….…30
3.4.4.2. Mott-Schottky…………………………………………………..……...31
3.4.4.3. 交流阻抗分析………………………………………………..…...…..32
第四章、 結果與討論…………………………………………………………34
4.1. 氧化鐵靶材製備參數研究……………………………………………….34
4.1.1. 粉末壓制靶材之壓力對靶材影響……………………………………..35
4.1.2. 靶材燒結之溫度對靶材影響…………………………………………..35
4.2. 脈衝雷射濺鍍沉積法製備氧化鐵薄膜研究…………………………….37
4.2.1. 雷射通量對薄膜之影響………………………………………………..38
4.2.2. 濺鍍沉積之氣氛對薄膜之影響………………………………………..42
4.3. 熱處理參數研究………………………………………………………….48
4.3.1. 熱處理溫度對薄膜影響………………………………………………..48
4.3.2. 熱處理氣氛對薄膜影響………………………………………………..54
4.4. 脈衝雷射濺鍍沉積時間對薄膜影響…………………………………….56
第五章、 結論與建議…………………………………………………………61
5.1. 結論……………………………………………………………………….61
5.2. 未來工作建議…………………………………………………………….62
文獻參考……………………………………………………………………….63
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