製備以含鈦混合氧化物PtRu觸媒及其在含CO氫氣電化學氧化之研究

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研究生：	楊智翔 Chih-Xsiang Yang
論文名稱：	製備以含鈦混合氧化物PtRu觸媒及其在含CO氫氣電化學氧化之研究 Preparation of Titanium mixed oxide supported Pt Ru catalysts for Hydrogen Electrochemical Oxidation Reaction of CO/H2
指導教授：	林昇佃 Shawn-D. Lin
口試委員:	黃炳照 Bing-Joe Hwang 林修正 Andrew-S. Lin
學位類別：	碩士 Master
系所名稱：	工程學院 - 化學工程系 Department of Chemical Engineering
論文出版年：	2020
畢業學年度：	108
語文別：	中文
論文頁數：	199
中文關鍵詞：	含鈦混合氧化物、鈣鈦礦、乙二醇還原法、氫氣氧化反應、CO耐受性
外文關鍵詞：	Titanium mixed oxide, Perovskite, Ethylene glycol method, hydrogen oxidation reaction, CO tolerance
相關次數：	點閱：238 下載：2
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本研究探討含鈦混合氧化物載體製作PtRu觸媒，作為H2燃料電池陽極並分析其氫氣氧化活性與CO耐受性，混合氧化物載體的導電性不如傳統碳黑載體，但其潛在優勢為穩定性較碳黑高。實驗室先前探討含鈦釕混合氧化物載體，在擔載Pt的過程中，會有部分Ru還原析出，並可進一步與Pt形成Pt-Ru合金相，但對生成Pt-Ru合金相的組成結構不易控制，本研究探討改善混合氧化物擔載Pt-Ru合金觸媒的製備。首先測試前處理條件對實驗室先前製作Ti0.7Ru0.3O2載體的影響，進一步調整Pt與PtRu的擔載參數。其次為含鈦之鈷鎳鈣鈦礦混合金屬氧化物(CoTiO3、NiTiO3)，具有高介電性質、特殊的電子結構且對CO、烴類等完全氧化有良好的活性，故將其擔載金屬並進一步優化調整PtRu的擔載比例，了解觸媒中各成分可能扮演的角色，及其對電化學反應特性與抗CO毒化的影響。
研究結果顯示經前處理之Ti0.7Ru0.3O2-C650載體有良好的結構穩定性，在擔載Pt過程中Ru不易還原析出，並透過調整PtRu的擔載參數擔所製20Pt10Ru/Ti0.7Ru0.3O2-C650 觸媒其PtRu合金粒徑約2奈米，分析顯示CO氧化起始電位低於20Pt10Ru/C-JM商用觸媒，氫氣氧化反應(HOR)在純氫、250和500 ppm CO/H2環境下的旋轉圓盤電極分析也具有良好的氫氣氧化活性與穩定性。含鈦之鎳鈷混合氧化物CoTiO3-1000及NiTiO3-1000載體經優化調整PtRu的擔載比例後所製的30Pt15Ru/CoTiO3-1000、 40Pt20Ru/CoTiO3-1000觸媒及 30Pt15Ru/NiTiO3-1000觸媒，亦有約2奈米之PtRu合金粒徑，具有低於商用觸媒的CO氧化電位、良好的氫氣氧化活性與穩定性，在長時間CO耐受性測試中，30Pt15Ru/CoTiO3-1000觸媒具有最好的CO容忍度表現。

This study explores the production of PtRu catalysts containing Titanium mixed oxide supports as H2 fuel cell anodes and analyzes Hydrogen electrochemical Oxidation activity and CO tolerance. The conductivity of mixed oxide supports are not as good as carbon supports, but its potential advantage is that it is more stable than Carbon supports. The laboratory previously discussed the Titanium-Ruthenium mixed oxide support, during the process of loading Pt, part of Ru will be reduced and precipitated, and it can further form a Pt-Ru alloy phase with Pt, but that the composition structure of the Pt-Ru alloy phase is hard to control. To discuss the improvement of the preparation of mixed oxide supported Pt-Ru alloy catalyst. First, test the effect of pre-processing conditions on the Ti0.7Ru0.3O2, and further adjust the loading parameters of Pt or PtRu. The second is Titanium-Cobalt (or Titanium-Nickel) perovskite oxides supports (CoTiO3, NiTiO3), which have high dielectric properties, special electronic structure and good activity for the complete oxidation of CO and hydrocarbons, and further optimizely adjust the loading ratio of PtRu content to understand the possible role of each component in the catalyst and its influence on the electrochemical reaction characteristics and resistance to CO poisoning.
The research results show that the pre-treated Ti0.7Ru0.3O2-C650 support has better structural stability, and Ru element is not easy to be reduced during the loading Pt process, and the 20Pt10Ru/Ti0.7Ru0.3O2-C650 catalyst has PtRu alloy particle size of about 2 nanometers. Analysis shows that the CO oxidation onset potential is lower than Commercial catalyst (20Pt10Ru/C-JM). And it has better hydrogen oxidation activity and stability with the rotating disk electrode (RDE) analysis by the hydrogen oxidation reaction (HOR) in pure hydrogen, 250 and 500 ppm CO/H2. With CoTiO3-1000 and NiTiO3-1000 as supports loading ratio of PtRu, 30Pt15Ru/CoTiO3-1000, 40Pt20Ru/CoTiO3-1000 and 30Pt15Ru/NiTiO3-1000 catalys are also the PtRu alloy particle size of about 2 nanometers, which has a lower CO oxidation potential than commercial catalysts (20Pt10Ru/C-JM), and better hydrogen oxidation activity and stability. At last, in the long-term CO tolerance test, 30Pt15Ru/CoTiO3-1000 catalyst has the best CO tolerance performance.

摘要            I
Abstract        III
致謝            V
圖目錄            X
表目錄            XIII
第1章、    緒論    1
1    前言    1
2    燃料電池    3
2.1    質子交換薄膜燃料電池 (PEMFC)    3
2.2    直接甲醇燃料電池 (DMFC)    5
3    文獻回顧    6
3.1    碳載體觸媒    7
3.2    金屬氧化物載體    9
3.2.1    氧化鈦 (Titanium oxides、TiOx)    10
3.2.2    氧化釕 (Ruthenium oxides、RuOx)    13
3.2.3    鈣鈦礦結構 (Pervoskite, ABO3)    14
3.2.4    混合金屬氧化物    16
3.3    Pt金屬觸媒    17
3.3.1    二元合金觸媒    18
3.3.2    多元合金觸媒    18
4    研究目的與方法    19
第2章、    研究設備與方法    20
1    研究架構    20
2    實驗藥品與設備    22
2.1    實驗藥品與氣體    22
2.2    實驗設備    23
3    觸媒載體製備方法    24
3.1    水熱法製備TiO2載體    24
3.2    水熱法製備Ti0.7Ru0.3O2載體    25
3.3    共沉澱法製備CoTiO3(或NiTiO3)載體    26
4    乙二醇還原法擔載Pt金屬觸媒    27
4.1    製備40wt%Pt金屬觸媒    27
4.2    製備20wt%Pt - 10wt%Ru、30wt%Pt - 15wt%Ru、40wt%Pt - 20wt%Ru合金觸媒    28
5    材料鑑定方法    29
5.1    X光繞射分析(XRD)    29
5.2    表面積與孔隙度測定儀 (BET)    30
5.3    掃描式電子顯微鏡-能量散射光譜儀 (SEM-EDS)    31
5.4    感應耦合電漿原子放射光譜儀 (ICP-AES)    32
5.5    X光吸收光譜 (XANES)    32
6    電化學分析方法    34
6.1    薄膜電極的製備    34
6.2    可逆氫電極(RHE)的前置作業    35
6.3    循環伏安法 (Cyclic voltammetry)    35
6.4    CO電催化氧化分析 (CO-stripping)    35
6.5    氫氣氧化反應之陽極測試條件 (HOR-pure H2)    36
6.6    氫氣氧化反應之陽極測試條件(HOR-250 or   500ppmCO/H2)    36
6.7    CO耐受性測試條件(PureH2 or 250ppmCO/H2)    37
6.8    電化學活性表面積與CO/H比例計算    38
6.9    塔弗方程式 (Tafel equation)    39
6.10    氫氣氧化之分析方法    39
第3章、    結果與討論    41
1    不同前處理Ti0.7Ru0.3O2載體擔載40%Pt觸媒    42
1.1    載體與觸媒特性分析    42
1.1.1    XRD分析    42
1.1.2    氮氣等溫吸/脫附分析及孔徑參數分析    49
1.1.3    材料之形貌及組成分析    53
1.2    不同前處理載體擔載40%Pt觸媒之電化學反應特性分析    58
1.2.1    觸媒之循環伏安法分析    58
1.2.2    觸媒之CO氧化脫除分析    60
1.2.3    不同前處理載體擔載40%Pt觸媒之氫氣氧化反應分析    64
2    調整Pt-Ru擔載參數對製成觸媒的影響    71
2.1    載體與觸媒特性分析    72
2.1.1    XRD分析    72
2.1.2    氮氣等溫吸/脫附分析及孔徑參數分析    76
2.1.3    材料之形貌及組成分析    80
2.2    擔載Pt-Ru金屬製成觸媒之電化學反應特性分析    85
2.2.1    觸媒之循環伏安法分析    85
2.2.2    觸媒之CO氧化脫除分析    87
2.2.3    擔載Pt-Ru金屬製成觸媒之氫氣氧化反應分析    91
3    含鈦鈣鈦礦載體擔載PtRu觸媒的特性    98
3.1    載體與觸媒特性分析    98
3.1.1    XRD分析    98
3.1.2    氮氣等溫吸/脫附分析及孔徑參數分析    104
3.1.3    材料之形貌及組成分析    108
3.1.4    CoTiO3-1000載體擔載PtRu製成觸媒Co-K edge之XANES圖譜        114
3.1.5    NiTiO3-1000載體擔載PtRu製成觸媒Ni-K edge之XANES圖譜        117
3.1.6    鈣鈦礦載體擔載PtRu製成觸媒Pt-L3 edge之XANES圖譜    120
3.1.7    鈣鈦礦載體擔載PtRu製成觸媒Ru-K edge之XANES圖譜    124
3.2    含鈦鈣鈦礦載體擔載PtRu觸媒之電化學反應特性分析    128
3.2.1    觸媒之循環伏安法分析    128
3.2.2    觸媒之CO氧化脫除分析    132
3.2.3    鈣鈦礦載體擔載PtRu觸媒之氫氣氧化反應分析    135
4    觸媒穩定度測試    144
第4章、    結論    148
第5章、    參考文獻    150
附錄A Nafion 厚度計算    156
附錄B 氫氣氧化動力學數據處理    157
附錄C 改良觸媒的影響    170
C.1 載體與觸媒特性分析    170
C.1.1 XRD分析    170
C.1.2 氮氣等溫吸/脫附分析及孔徑參數分析    173
C.2 Ti0.7Ru0.3O2-c650擔載Pt-Ru觸媒之電化學反應特性分析    175
C.2.1 觸媒之CO氧化脫除分析    175
C.2.3 Ti0.7Ru0.3O2-c650擔載Pt-Ru觸媒之氫氣氧化反應分析    177
附錄D  EXAFS參數分析結果    180

                                

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