臺灣博碩士論文加值系統

光催化還原CO2成碳氫化合物燃料已經受到越來越多的關注，因為這個策略奏效可以減少溫室氣體之排放和提供替代能源之應用。雖然一些金屬氧化物和非金屬氧化物已被廣泛作為光催化劑，它們在光催化還原CO2反應中的效率仍然是非常低，無法產生經濟效益。亟需要能開發高效率性光觸媒系統應用於光催化還原CO2。本研究利用氧化石墨烯(GO)製備Z-Scheme奈米異質系統的光觸媒，利用不同的處理方式形成Ag2O/Ag/GO Z-Scheme組成結構，提高高電荷分離效率和強烈的氧化還原能力。運用X射線粉末繞射儀(XRD)、穿透式電子顯微鏡(TEM)、高解析X光光電子能譜儀(HR-XPS)、紫外光-可見光漫反射分光光譜儀（UV-Vis DRS）、比表面積分析儀(BET)、螢光光譜儀(PL)、傅立葉轉換紅外線光譜儀(FTIR)及熱重損失分析儀(TGA)鑑定其Ag2O/Ag/GO奈米組成、能隙大小及化合物的結構狀態資訊。最後利用光催化還原CO2，進行觸媒活性測試甲醇之產生速率，並得知在鍛燒溫度300℃及鍛燒時間1hr之5wt% Ag2O/Ag/GO光觸媒，甲醇產生速率為最高，其計算出RMeOH =8.6x105μmole g-cat-1hr-1。
另外利用高解析度電子顯微鏡分析光觸媒5wt% Ag2O/Ag/GO之晶體內部結構及晶面間距，確認Ago和Ag+1的同時存在。因此我們提出了Z-Scheme反應機制，Ag2O/Ag/GO光催化反應過程中，Ago可作為電荷傳輸介質，這類型的電荷轉移有效地增強了電子-電洞的分離，在紫外光的照射下，Ag2O和GO受光激發分別在導帶(CB)和價帶(VB)產生電子(e-)和電洞(h+)，Ag2O中導帶上的光激發電子通過Ago轉移到GO的價帶中，過程中Ag2O價帶位置的電洞會進行氧化反應，具有很強的氧化能力,可以分解H2O釋放出H2 + O2，GO導帶位置的電子則會與外界進行還原反應，具有高的還原能力，將CO2還原得到甲醇(CH3OH)，能大幅提升二氧化碳光催化還原成甲醇的效率。

Photocatalytic reduction of CO2 is a promising technology to both reduces the greenhouse gas emissions and provides alternative energy sources. Here, we designed a hierarchical Z-scheme photocatalyst consists in an Ag2O/Ag/GO nanostructure, in which Ag was deposited on the GO and subsequently Ag2O was oxidized on the surface of Ag/GO. Transmission Electron Microscopy (TEM), X-ray Diffractometer (XRD), X-ray Photoelectron Spectroscopy (XPS), UV-vis Diffuse Reflectance Spectra (UV-vis DRS), Surface Area and Porosity Analyzer (BET), Fluorescence Spectrophotometer (PL), Thermogravimetric analyzer (TGA) and Fourier transform infrared spectroscopy (FTIR) analysis were applied to characterize the Ag2O/Ag/GO catalysts. In addition, the photocatalytic activities of the Ag2O/Ag/GO catalysts were evaluated by the photocatalytic reduction of CO2 to methanol. The maximum MeOH formation rate was reached at a 0.01gram of 5wt% Ag2O/Ag/GO composite catalyst and a 300 mL of 0.2 N NaOH under the UV irradiation. The results of this reaction conditions have shown the methanol formation rate of 8.6 x105μmole g-cat-1hr-1.
From the results, the HRTEM image clearly indicates an intimate interface between Ag2O, Ag and GO in the composite and some lattice fringes can be clearly observed. The lattice spacing of 0.23 nm and 0.271 nm match the (111) plane of Ag and the (111) plane of Ag2O, respectively. We have proposed a possible Z-scheme mechanism based on the results. Z-scheme consists of ultrathin graphene oxide plates and Ag2O nanoparticles as photocatalysts, and Ag nanoparticle as a solid electron mediator offering a high speed charge transfer channel and leading to more efficient spatial separation of electron-hole pairs. It allows the electrons remaining in the conduction band (CB) of GO and holes in the valence band (VB) of Ag2O to possess strong reduction and oxidation capabilites, respectively, leading the Ag2O/Ag/GO to exhibit high photocatalytic reduction of CO2.

摘要 i
Abstract iii
目錄 v
表目錄 ix
圖目錄 x
第一章 緒論 1
1-1 前言 1
1-2 研究目的 3
第二章 文獻回顧 5
2-1 光觸媒之介紹與發展 5
2-1-1 光觸媒的基本原理 6
2-1-2 光觸媒的反應機制 7
2-2 光催化還原二氧化碳 10
2-2-1 二氧化碳回收處理方式 10
2-2-2 光催化還原二氧化碳機制 11
2-3 光觸媒效率之提升 16
2-3-1 異質接面改質光觸媒 17
2-3-2 添加貴重金屬 19
2-3-3 光觸媒之結構 21
2-3-4 光敏化光觸媒 23
2-3-5 Z-Scheme機制 25
2-4 石墨烯簡介 28
2-4-1 石墨烯之製備方法 30
2-4-2 氧化石墨烯應用於光催化還原二氧化碳之文獻探討 32
2-5 銀系半導體光觸媒 38
2-5-1 氧化銀光觸媒 39
2-5-2 銀系光觸媒應用於光催化還原二氧化碳之文獻探討. 40
第三章 實驗設備與研究方法 42
3-1 實驗藥品 42
3-2 實驗儀器 43
3-3 觸媒材料之製備 45
3-3-1 氧化石墨烯 (Graphene Oxide，GO)製備 45
3-3-2 Ag2O/ Ag/ GO 觸媒製備 47
3-4 儀器分析原理簡介 49
3-4-1 穿透式電子顯微鏡 (TEM) 49
3-4-2 高解析X光繞射儀 (XRD) 51
3-4-3 熱重損失分析儀 (TGA) 53
3-4-4 比表面積與孔洞分析儀 (BET) 55
3-4-5 傅立葉轉換紅外線光譜儀 (FTIR) 59
3-4-6 紫外光/可見光光譜儀 (UV-Vis) 61
3-4-7 X-射線光電子光譜 (XPS) 63
3-4-8 紫外光/可見光漫反射分光光譜儀 (DRS) 64
3-4-9 螢光光譜儀 (PL) 65
3-4-10 拉曼光譜儀 (Raman) 66
3-4-11 氣相層析儀 (GC-FID) 67
3-5 二氧化碳光催化還原反應 70
3-5-1 GC-FID操作條件 72
3-5-2 產物的定性 73
3-5-3 產物的定量 74
第四章 實驗結果與討論 75
4-1 氧化石墨烯(Graphene Oxide，GO)之特性分析 75
4-1-1 BET分析 75
4-1-2 XRD分析 77
4-1-3 TEM分析 78
4-1-4 FTIR分析 80
4-1-5 Raman分析 81
4-1-6 XPS分析 83
4-1-7 TGA分析 85
4-2 奈米銀擔持於氧化石墨烯之特性分析 86
4-2-1 不同比例的奈米銀擔持於氧化石墨烯之特性分析 86
4-2-1-1 XRD分析 86
4-2-1-2 TEM分析 87
4-2-1-3 UV-vis分析 90
4-2-1-4 FTIR分析 91
4-2-1-5 Raman分析 92
4-2-1-6 XPS分析 93
4-2-1-7 TGA分析 98
4-2-1-8 UV-Vis DRS分析 100
4-2-2 不同鍛燒溫度的奈米銀擔持於氧化石墨烯之特性分析 …………………………………………………………101
4-2-2-1 XRD分析 101
4-2-2-2 FTIR分析 103
4-2-2-3 Raman分析 105
4-2-2-4 UV-Vis DRS分析 106
4-2-3 不同鍛燒時間的奈米銀擔持於氧化石墨烯之特性分析 …………………………………………………………107
4-2-3-1 XRD分析 107
4-2-3-2 FTIR分析 109
4-2-3-3 Raman分析 110
4-2-3-4 UV-Vis DRS分析 111
4-3 奈米銀擔持於氧化石墨烯之光催化還原二氧化碳反應 112
4-3-1 氧化石墨烯和石墨烯之GC分析 113
氧化石墨烯和石墨烯之PL分析 115
4-3-2 不同比例的奈米銀擔持於氧化石墨烯之GC分析 116
不同比例的奈米銀擔持於氧化石墨烯之PL分析 118
4-3-3 不同鍛燒溫度的奈米銀擔持於氧化石墨烯之GC分析 …………………………………………………………119
不同鍛燒溫度的奈米銀擔持於氧化石墨烯之PL分析 121
4-3-4 不同鍛燒時間的奈米銀擔持於氧化石墨烯之GC分析 …………………………………………………………122
不同鍛燒時間的奈米銀擔持於氧化石墨烯之PL分析 123
4-3-5 不同5wt%Ag2O/Ag/GO的觸媒量克數之GC分析 124
4-4 Z-scheme系統之反應機制 125
HRTEM 127
第五章 結論 128
參考文獻 130
附錄 138

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