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研究生： 許又瑄
Hsu, Yu-Hsuan
論文名稱： 優化(鉬修飾)鉑鈷觸媒之製程應用於真實質子交換膜燃料電池
Optimization of (molybdenum-modified) platinum-cobalt catalyst process for real proton exchange membrane fuel cells.
指導教授： 潘詠庭
Pan, Yung-Tin
口試委員: 林育正
Lin, Yu-Jeng
吳子和
Wu, Tzu-Ho
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： 2023
畢業學年度： 111
語文別： 中文
論文頁數： 104
中文關鍵詞： 燃料電池 、鉑鈷觸媒 、介金屬結構 、製程優化
外文關鍵詞： Fuel cell, PtCo catalyst, Intermetallic structure, Process optimization
相關次數： 點閱：149  下載：0 
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    • 石化燃油燃燒產生的廢氣所致溫室氣體，各國開始尋求乾淨且具經濟效益的替代能源，氫燃料電池的產物水為未來最具潛力的能源轉換系統。氫燃料電池的鉑觸媒已經普遍被使用於質子交換膜燃料電池 (Proton-Exchange Membrane Fuel Cells, PEMFC)。然而，價格高昂一直是生產成本無法降低的主要原因。觸媒以富含鉑金屬，利用地球含量高的過渡金屬(Fe，Co，Ni)形成合金已經是眾多研究團隊有效降低鉑使用率的方式。基於成本考量，低負載鉑燃料電池觸媒在實際應用中，特別對於氧還原反應 (Oxygen Reduction Reaction, ORR) ，仍然是一個研究的課題。然而，在實際燃料電池測試條件下，通過旋轉圓盤電極 (Rotating Disk Electrode, RDE) 測試條件獲得的高性能可能無法轉移到膜電極組件上。本研究通過改進鉬摻雜金屬鉑鈷觸媒的製備來解決這一問題，並縮小旋轉圓盤電極和膜電極 (Membrane Electrode Assemblies, MEA) 測試系統之間的差距。從先前的研究中，我們發現在觸媒表面摻雜鉬可以提高鉑鈷觸媒在旋轉圓盤電極條件下的性能和耐久性[1]。通過循環伏安法進行多次的預處理，以去除覆蓋觸媒表面活性位點過量的鉬。首先透過使用鹼溶液去除多餘的鉬，但是鹼的殘留不利於膜電極測試。因此，我們透過直接減少鉬的使用來修改鉬的摻雜過程，省略使用強鹼的步驟，這樣的方式提升觸媒在燃料電池中的表現也更容易用於商業生產。更進一步，為了解決貴金屬觸媒利用率的問題，我們利用較高比表面積的碳製備鉑鈷觸媒，探討觸媒載體在乙二醇還原法對於鉑金鈷觸媒的差異，並合成出分散性與奈米粒子更小的鉑鈷觸媒，這方法不僅便宜方便、適合商業化生產，在不使用高分子化學封端劑的條件下，也達到了綠色能源的目標。

    The greenhouse gases generated by the combustion of petrochemical fuels have prompted countries to seek clean and economically viable alternative energy sources. Hydrogen fuel cells, with water as the product, are considered the most promising energy conversion system for the future. Platinum catalysts in proton-exchange membrane fuel cells (PEMFC) have been widely used. However, the high cost has been a major obstacle to reducing production costs. One effective way to reduce platinum usage is through alloying with abundant transition metals (Fe, Co, Ni) with high Earth abundance. Considering cost, low-loading platinum fuel cell catalysts, especially for the oxygen reduction reaction (ORR), remain a research challenge in practical applications. However, achieving high performance obtained under rotating disk electrode (RDE) conditions in real fuel cell tests may be challenging to transfer to membrane electrode assemblies (MEA). In this study, we addressed this issue by improving the preparation of molybdenum-doped platinum-cobalt catalysts and narrowing the gap between RDE and MEA testing systems. Previous research has shown that molybdenum doping on the catalyst surface can enhance the performance and durability of platinum-cobalt catalysts under RDE conditions. Excessive molybdenum on the catalyst surface was removed through multiple cycles of pre-treatment using cyclic voltammetry. Initially, excess molybdenum was removed using an alkaline solution, but the residue of alkali was detrimental to MEA testing. Therefore, we modified the molybdenum doping process by reducing the use of alkaline solutions, making it more suitable for commercial production. Furthermore, to address the issue of precious metal catalyst utilization, we used carbon with a higher specific surface area to prepare platinum-cobalt catalysts, investigating the differences in catalyst support through the ethylene glycol reduction method. This allowed us to synthesize platinum-cobalt catalysts with improved dispersion and smaller nanoparticles. This approach is not only cost-effective and convenient for commercial production but also aligned with the goal of green energy without the need for polymer chemical capping agents.

    摘要..........................................................I Abstract.....................................................II 目錄.........................................................IV 圖目錄.......................................................VII 表目錄........................................................XI 第一章 緒論....................................................1 第二章 文獻回顧................................................2 2.1引言.......................................................2 2.2質子交換膜燃料電池組........................................3 2.3質子交換膜燃料電池工作原理...................................4 2.3.1陰極氧還原反應機制........................................6 2.3.2提升氧還原反應觸媒........................................7 2.4陰極觸媒材料................................................9 2.4.1以鉑為基礎金屬觸媒種類.....................................9 2.4.2觸媒合金與結構(核殼結構、金屬間有序結構)....................10 2.4.3鉑系列觸媒製備方法........................................13 2.4.4如何降低鉑鈷觸媒高溫燒結方法...............................16 2.4.5觸媒載體的碳材種類........................................22 2.5旋轉圓盤電極與燃料電池之間的差距.............................23 2.6研究動機...................................................27 第三章 實驗方法及步驟..........................................31 3.1實驗藥品...................................................31 3.2實驗儀器...................................................33 3.3實驗方法...................................................35 3.3.1 PtCoMo觸媒製備..........................................35 3.3.2 乙二醇還原法將PtCo觸媒合成於不同碳材......................37 3.3.3膜電極製作...............................................38 3.4觸媒及膜電極特性分析方法....................................39 3.4.1 X光粉末繞射(X-ray Powder Diffractometer, XRD)...........39 3.4.2穿透式電子顯微鏡(Transmission Electron Microscope, TEM)...40 3.4.3熱重分析儀(Thermogravimetric Analyzer, TGA)..............40 3.4.4拉曼光譜(Micro Raman Identify Dual, MRID)................41 3.4.5 感應耦合電漿發散光譜儀(Inductively Coupled Plasma Optical Emission, ICP-OES)...........................................41 3.4.6 表面積與孔洞分析儀(BET)..................................42 3.4.7 高解析x射線光電子能譜儀(High Resolution X-ray Photoelectron Spectroscope, HRXPS).........................................43 3.4.8 膜電極電化學特性測量.....................................43 第四章 結果與討論..............................................45 4.1PtCoMo觸媒材料特性鑑定與燃料電池應用.........................45 4.1.1鉑鈷觸媒合金與有序程度....................................45 4.1.2鉑鈷觸媒於碳材分佈情況....................................47 4.1.3金屬觸媒鉑鈷定量分析......................................48 4.1.4電化學表現討論............................................50 4.2 PtCoMo觸媒針對PtCo核製程改善...............................55 4.2.1碳材的特性對於PtCo觸媒合成的影響...........................55 4.2.2 PtCo合成於Vulcan結果分析.................................61 4.2.2.1 含浸法對PtCo合成於Vulcan上之XRD分析.....................61 4.2.2.2不同比例Co前驅物對PtCo合成於Vulcan上之XRD分析.............62 4.2.2.3不同比例Co前驅物對PtCo合成於Vulcan上之定量分析............64 4.2.2.4不同比例Co前驅物對PtCo合成於Vulcan上之TEM分析.............66 4.2.3 PtCo合成於不同碳材 (Vulcan XC-72R、Ketjen EC600J、Black Pearl 2000) 結果討論.................................................70 4.2.4 PtCo降低鈷前驅物比例合成於Ketjen、BP2000..................77 第五章 結論....................................................83 第六章 未來工作.................................................85 6.1 PtCo動力學控制合成於Ketjen..................................85 6.2 燃料電池測試................................................92 6.3 MNC 結構做為載體............................................94 附錄...........................................................94 參考文獻........................................................97

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