根據先前的研究結果，銀奈米粒子/氧化鐵/還原石墨烯(Ag/FNG)，三者之界面對氧氣還原反應的活性有很大的幫助。我們更進一步地配合特定波長之雷射(405 nm)，發現有抑制中間產物過氧化物的現象，但是對於催化劑進行氧氣還原反應的機制，並沒有詳細的研究，因此我們使用電化學阻抗頻譜法(Electrochemistry Impedance Spectroscopy, EIS)與光電壓衰減法(Potovoltage decay來探討進行氧氣還原反應與光電子之電荷轉移情形。
照射405 nm雷射後，過氧化氫抑制量為7.5%，且光電壓衰減結果顯示Ag/FNG有比較少的陷阱狀態(trap state)，對於光/電化學催化有比較好的催化表現。另一方面催化劑之光活性來自於照光時，銀奈米粒子產生表面電漿共振之熱電子與氧化鐵之光電子皆轉移到氧化鐵之導電能帶，使催化劑表面擁有較豐富的電子，推測是造成活性上升的主因，且實驗結果顯示光照使催化劑產生較多的活性點，可以還原較多的氧氣，得到比較大的還原電流，有更好的氧氣還原活性。

According to the previous research results, silver nanoparticles/iron oxide/N-doped graphene (Ag/FNG), the interface between each of them are very helpful for improving the oxygen reduction reaction activity. We further coupled with lasers with the specific wavelength (405 nm) and found that there was a phenomenon of suppressing the generation of peroxide. However, there was less study about the mechanism of the oxygen reduction reaction of catalysts, so we used the electrochemistry impedance spectroscopy (EIS) and photovoltage decay to investigate the effect of the oxygen reduction reaction and photoelectron charge transfer.
After irradiated with 405 nm laser, the percentage of hydrogen peroxide inhibition was 7.5%, and the results of photovoltage decay showed that the Ag/FNG had a relatively less trap state and had a better catalytic performance for laser-coupled oxygen reduction reaction. On the other hand, when the photoactivity of the catalyst arises from laser irradiation, the electrons generate by surface plasma resonance of the silver nanoparticles and the photoelectrons of the iron oxide would transfer to the conduction band of the iron oxide, so that the catalyst surface has abundant electrons. The main reason for the increase in activity is that the illumination makes the charge transfer between the catalyst and oxygen faster and the catalyst reacts more easily with oxygen, resulting in a larger reduction current density and better oxygen reduction activity.

目錄
論文審定書 i
致謝 ii
摘要 iii
Abstract iv
目錄 v
圖目錄 viii
表目錄 x
第一章、緒論 1
1.1 研究動機 2
1.2 研究背景 3
1.2.1 氧氣還原反應 3
1.2.2 氧氣親和力 4
1.2.3 氧氣還原反應催化劑 5
1.2.3.1 鉑催化劑 5
1.2.3.2 石墨烯催化劑 6
1.2.3.3 銀奈米粒子複合催化劑 8
1.2.3.4 氧化鐵複合催化劑 9
1.2.4 光催化劑 11
1.2.4.1 半導體 11
1.2.4.2 金屬之表面電漿共振 12
1.2.4.3 碳材料 14
1.2.4.4 光輔助氧氣還原反應 15
1.2.5 光輔助燃料電池 18
1.2.6 先前的研究 21
第二章、實驗樣品合成與測試方法 24
2.1 實驗藥品 24
2.2 合成 25
2.2.1 製備氧化石墨烯 (graphene oxide) 25
2.2.2 合成Ag/FNG(Ag/Fe2O3/N-Graphene) 25
2.2.3 合成FNG, Ag/N-rGO, Fe2O3 25
2.3 電化學量測 26
2.3.1 循環伏安法 (Cyclic voltammetry, CV) 26
2.3.2 旋轉環盤電極 (Rotation ring disk electrode, RRDE) 26
2.4 光輔助氧氣還原反應 27
2.5 電化學阻抗頻譜分析法 29
2.5.1 等效電路阻抗介紹 30
2.6 UV量測 31
2.7 UPS原理 31
2.8 曲線擬合 31
2.9 光電壓量測 32
第三章、研究結果 33
3.1 雷射波長選擇 33
3.2 光輔助氧氣還原反應 35
3.2.1 定電位量測雷射之影響 35
3.2.2 連續光源 38
3.2.3 光源對極限電流之影響 39
3.2.4 曲線擬合極限電流 40
3.2.5 光源對於還原行為之影響 42
3.2.6 不同功率雷射影響 44
3.2.7 未修飾催化劑之玻璃探電極(GCE)測試 45
3.3 電化學交流阻抗頻譜法 47
3.3.1 旋轉電極之催化行為 47
3.3.2 照光對於催化劑阻抗之影響 50
3.3.3 靜止電極之催化行為 52
3.4 光電壓衰減 55
3.4.1 一般條件 55
3.4.2 加入Fe(CN)63-/4-之影響 57
3.4.3 固定電壓差之光電壓衰減 58
第四章、綜合討論 59
4.1 光照機制探討 59
4.2 光輔助氧氣還原反應 60
4.3 在照光後的質傳增強行為 60
4.4 陷阱能態對電化學之影響 60
第五章、結論 62
參考文獻 63
附錄 70
 
圖目錄
圖 1 1 金屬對氧鍵結能與活性圖。 4
圖 1 2 Pt/C經過長時間的電催化反應會有四種不同降解途徑(A)為實驗前(B)為實驗後，藍色為Pt奈米粒子溶解，橙色為活性碳腐蝕，綠色為奈米粒子凝聚，紅色為奈米粒子從活性碳脫離。 5
圖 1 3 氮原子摻雜碳材料之不同氮類型。 6
圖 1 4 氮摻雜之碳材料氧氣還原反應機制。 7
圖 1 5 縮小銀奈米粒子之氧氣還原活性影響。 8
圖 1 6 氧化鐵與石墨烯複合材料，在ORR與OER之動力學表現。 10
圖 1 7 氧化鐵與石墨烯複合材料，在ORR之動力學表現。 10
圖 1 8 表面電漿共振之金屬，受激發之電子誘導氧分子解離之機制。 13
圖 1 9 多孔碳材料對於光引發氧氣還原電流增強。 14
圖 1 10 於AgPt合金照射光源之電流密度變化與過氧化氫抑制量。 16
圖 1 11 Au-Pd-Pt受光照射後，電流密度的變化。 16
圖 1 12 Au@TiO2對光引發起始電壓、電流密度、電子轉移數、過氧化氫產率變化。 17
圖 1 13 生物燃料電池兩極催化劑示意圖。 18
圖 1 14 燃料電池之半導體高分子之陰極材料，受光激發之電子轉移機制圖。 19
圖 1 15 光輔助氫氧燃料電池裝置圖，在陰極放置石英玻璃並照光。 20
圖 1 16 pTTh陰極催化劑與氧氣反應電荷轉移圖。 20
圖 1 17 催化劑示意圖(a) Ag/FNG、(b) FNG、(c) Ag/N-rGO 22
圖 1 18 各催化劑氧氣還原活性 (a)於1600 rpm動力學上的表現、(b) CV。 23
圖 2 1 空白電極校正(a) 為盤電流(b) 為環電流。 28
圖 2 2 光輔助氧氣還原反應裝置架設示意圖。 28
圖 2 3 左圖為未照光狀態，為電極受淺的(ets)以及深的(etd)表面狀態影響之費米能階的改變；右圖為照光後，產生之光電子電動對之開路電壓變化(∆V1, ∆V2)。 32
圖 3 1紫外光分光儀測試催化劑(Ag/FNG、Ag/N-rGO、FNG、rGO、Fe2O3)之吸收光譜。 34
圖 3 2 雷射照射各催化劑之氧氣還原反應(a) 盤電流密度變化、(b) 環電流變化、(c) 過氧化氫產率變化。 37
圖 3 3 使用連續光源照射催化劑之氧氣還原反應(a) 盤電流密度變化、(b) 環電流變化、(c) 過氧化氫產率變化。 38
圖 3 4 雷射照射Ag/FNG催化劑，電流密度之變化。 39
圖 3 5 Ag/FNG實驗與理論擬合圖譜 41
圖 3 6 照射雷射之CV(a) Ag/FNG、(b) Ag/N-rGO、(c) FNG。 43
圖 3 7 測試不同功率之雷射於Ag/FNG催化劑CV圖。 44
圖 3 8照光後催化劑的活化情形示意圖。 45
圖 3 9 測試未加入催化劑之空白電極，在飽和氧氣之0.1 M KOH中，於照射405 nm雷射5分鐘(a) CV、(b) LSV。 46
圖 3 10本文選用之等效電路圖。 49
圖 3 11各催化劑交流阻抗擬合結果。 49
圖 3 12 各催化劑照光之交流阻抗擬合結果(a) Ag/FNG、(b) Ag/N-rGO、(c) FNG。 51
圖 3 13 各催化劑照光之交流阻抗擬合結果(a) Ag/FNG、(b) Ag/N-rGO、(c) FNG。 54
圖 3 14 光電壓變化(a) 一般條件、(b) 加入Fe(CN)63-/4-。 57
圖 3 15 各催化劑固定電壓差之光電壓衰減。 58
圖 4 1 光輔助氧氣還原反應可能之電子轉移機制。 61
 
表目錄
表 1 1 各催化劑之ORR活性比較表 21
表 3 1 照射405 nm雷射電流密度變化、過氧化氫抑制量 36
表 3 2 各項係數說明 40
表 3 3 擬合參數結果 41
表 3 4 Ag/FNG、Ag/N-rGO、FNG之阻抗值。 48
表 3 5 照光對旋轉電極之阻抗影響 50
表 3 6 照光下對固定電極阻抗之影響 53
表 3 7 光電壓衰減之生命期計算 56
表 3 8 光電壓變化值 56
表 3 9 各催化劑固定電壓差光電壓衰減生命期之計算。 58

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