石墨烯為基材之複合材料於化學儲能及轉換系統之應用

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研究生：	劉芊良
論文名稱：	石墨烯為基材之複合材料於化學儲能及轉換系統之應用 Graphene-based Composite Materials in the Applications of Electrochemical Storage and Conversion Systems
指導教授：	胡啟章
口試委員:	張國興白育綸
學位類別：	碩士 Master
系所名稱：	工學院 - 化學工程學系 Department of Chemical Engineering
論文出版年：	2013
畢業學年度：	101
語文別：	英文
論文頁數：	118
中文關鍵詞：	石墨烯、氮摻雜、超電容、燃料電池
相關次數：	點閱：2 下載：0
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本研究主要是利用擁有大表面積、良好導電度和絕佳熱傳導性等各種優點的石墨烯與不同種類物質相互結合形成複合材料後，應用在超級電容器及氧氣還原方面。論文結果主要分為兩個部分。第一部分結果係利用一快速且簡單的實驗合成法製備石墨烯與錳氧化物的複合材料，並將其應用在超級電容器上。第二部分則是利用實驗設計法(DOE)分析將含氮化合物摻入石墨烯內所得到的氮摻雜石墨烯複合材料於何種實驗條件下，可以獲得接近2個電子轉移或是4個電子轉移的氧氣還原能力。以下將簡要地討論兩章所包含的內容。
第一部分藉由微波輔助水熱法(MAHS)製備四氧化三錳(Mn3O4)與石墨烯(graphene)之奈米複合材料(nanocomposites)，作為對稱型及非對稱型超級電容器之電極材料，並有系統地探討四氧化三錳(Mn3O4)含量對於複合材料的微結構及電化學表現之影響。此外，也利用掃瞄式電子顯微鏡(SEM)、X光繞射儀(XRD)及熱重量分析儀(TGA)分析複合材料的表面形貌、錳氧化物的結晶結構及複合材料中石墨烯(graphene)之含量。結果顯示，錳氧化物含量為82.4重量百分比的複合材料(GMn80)具有最佳的電容效果(~193 F/g)，因而進一步利用此混合比例的複合材料作為測試對稱型及非對稱型超級電容器的電極材料。實驗結果可知，藉著組合由GMn80所做成的陰極電極與利用微波輔助水熱法合成的氮摻雜石墨烯做成的陽極電極而成的非對稱型超級電容器，擁有高達2V的操作電位窗，並能在24 A/g的電流密度下，展現11.11 Wh/kg的能量密度及23.5 kW/kg的功率密度。
第二部分則同樣利用微波輔助水熱法(MAHS)製備氮摻雜石墨烯複合材料，並應用在氧氣還原上。由於金屬空氣電池和光電化學催化分解有機物的兩大重要應用下，我們透過實驗設計法(Design and analysis of Experiments, DOE)分析吡咯(Pyrrole)單體濃度(A)、微波功率(B)、微波反應溫度(C)和微波持溫時間(D)等四個實驗條件何者對於氧氣還原之電子轉移數目影響較大。實驗結果顯示，以微波功率(B)和微波反應溫度(C)最能夠影響氮摻雜石墨烯的氧氣還原效果。而在陡升實驗和陡降實驗當中，透過改變微波功率(B)和微波反應溫度(C)的條件，我們可以有效控制氮摻雜石墨烯的電子轉移數目從2.6至3.8，此結果對於需要進行2個電子轉移反應而產生雙氧水(H2O2)以光電化學催化有機物的應用和需要接近4個電子轉移反應的金屬空氣電池有很大助力。另外，透過X射線光電子能譜儀(XPS)分析，我們確定吡咯型的氮結構(pyrrolic-nitrogen structure)是影響氮摻雜石墨烯氧氣還原效果的主要因素。

中文摘要    IV
Abstract    III
Table of Contents    VIII
List of Figures    XII
List of Tables    XVII
Chapter 1 Introduction and Literature Review    1
1 Fundamentals of Electrochemistry    1
1.1 Electrochemical System and Reference Electrodes    1
1.2 Faradic and Non-faradic Processes    6
1.3 Electrochemical Cells and Reaction Rate    7
1.4 Factors Affecting Electrode Reaction Rate and Current    10
1.5 Factors Affecting Electrochemical System    11
2 Introduction of Microwave-assisted Hydrothermal/Solvothermal Synthesis (MAH/MAS)    12
3 Introduction of Design and Analysis of Experiments (DOE)    17
4 Brief Review of Graphene and its Applications    21
4.1 Introduction of Graphene: A Cutting-edge Material    21
4.2 Introduction of Manganese Oxide/Graphene    25
4.3 Introduction of Nitrogen-doped Graphene    31
4.3.1 N-doped Structures in Carbon Materials    31
4.3.2 N-doped Graphene as the Catalyst for ORR in Fuel Cells    32
5 Motives    36
Chapter 2 Experimental Methods    37
1 Chemicals and Instruments    37
1.1 Chemicals    37
1.1.1 Mn3O4/Graphene    37
1.1.2 Nitrogen-doped Graphene    38
1.2 Instruments    39
1.2.1 Mn3O4/Graphene    39
1.2.2 Nitrogen-doped Graphene    40
2 Graphite Substrate Pretreatments    41
3 Electrode preparation    41
4 Preparation of Graphite Oxide    42
5 Mn3O4/Graphene Composite Material    43
5.1 Preparation of Mn3O4/Graphene Composite Material    43
5.2 Preparation of N-doped Graphene    43
5.3 Material Characterization of Mn3O4/Graphene Composites    44
5.4 Electrochemical Analysis    44
6 Nitrogen-doped Graphene Composite Material    46
6.1 Preparation of Nitrogen-doped Graphene Composite Material    46
6.2 Material Characterization of Nitrogen-doped Graphene Composites    46
6.3 Electrochemical Analysis    46
Chapter 3 Mn3O4/graphene Composite Material    49
1 Introduction and Motive    49
2 Textural Analysis of Mn3O4/Graphene Composites    49
3 Effects of Different Mixing Ratio of Mn3O4/Graphene Composites on Electrochemical Performances    57
4 Performances of Symmetrical and Asymmetrical Supercapacitors    65
4.1 Performances of Symmetrical Supercapacitors    65
4.2 Performances of Asymmetrical Supercapacitors    68
5 Conclusions    72
Chapter 4 Nitrogen-doped Graphene Composite Material    73
1 Introduction and Motive    73
2 Design of Experiments for the application of Fuel Cells    75
2.1 Qualitatively descriptions for the RRDE responses of N-doped Graphene    75
2.2 Full factorial design    79
2.3 Path of the Steepest Ascent and Descent Study    90
3 Textural Analysis of Nitrogen-doped Graphene    93
4 Conclusions    96
Chapter 5 Conclusions and Future Work    97
1 Conclusions and Future Work of Mn3O4/graphene Composite Material    97
2 Conclusions and Future Work of Nitrogen-doped Graphene Composite Material    99
3 Future Work of Graphene-based Composite Material    100
References    101

                                

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