鎵化鉑、鎵化鈀和鉑化錫奈米合金材料之合成與其應用於電催化反應的研究

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研究生：	林淑娟 Lim, Suh-Ciuan
論文名稱：	鎵化鉑、鎵化鈀和鉑化錫奈米合金材料之合成與其應用於電催化反應的研究 Synthesis of Gallium-Platinum, Gallium-Palladium and Platinum-Tin Nanomaterials for electrocatalytic applications
指導教授：	段興宇 Tuan, Hsing-Yu
口試委員:	周更生黃暄益曾院介張恕豪
學位類別：	博士 Doctor
系所名稱：	工學院 - 化學工程學系 Department of Chemical Engineering
論文出版年：	2018
畢業學年度：	107
語文別：	英文
論文頁數：	95
中文關鍵詞：	電化學觸媒、電解水產氫、燃料電池、鎵化鉑、鎵化鈀、鉑化錫
外文關鍵詞：	electrocatalysts, hydrogen evolution reaction, fuel cell, gallium-platinum, gallium-palladium, platinum-tin
相關次數：	點閱：3 下載：0
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發展高效能和穩定電化學觸媒用於電解水產氫和燃料電池，是綠色能源的一項重要課題。本論文主要研究貴金屬基奈米材料的合成與其電催化反應之應用，主要內容概括如下：（1）合成爆米花形鎵化鉑（GaPt3）奈米粒子及其作為電解水產氫反應（HER）電催化劑之應用（2）鎵化鈀（GaPd2）奈米材料的形態控制並應用於HER（3）厚度小於1 nm之鉑化錫（PtSn）奈米片用於甲醇和乙醇氧化反應（MOR和EOR）。
儘管HER的替代材料快速增長，但Pt基或Pt合金材料仍然是最有效的催化劑。我們採用熱溶劑合成法製備爆米花形GaPt3奈米顆粒具有間金屬特性，其凹凸不平的粗糙表面，為催化反應提供了較大的表面積使其反應活性增加。然而於HER中，GaPt3奈米粒子的電催化活性首次於本研究中進行評估。線性掃描伏安法結果表示GaPt3奈米粒子於酸性溶液中具有優於商業白金觸媒的卓越的電催化活性，僅需27mV過電位即可達到10 mA / cm2電流密度和43.3mV / dec的塔菲爾斜率。而在大工作面積 (5 cm2) 反應，電流密度10 mA/cm2下仍可維持相當低的過電位(<80 mV) 。接著做觸媒持久度的評估，GaPt3奈米粒子做為工作電極的催化反應，以伏安法進行10000次CV掃描（−0.3 to 0.2 V vs. RHE）和48小時 V的穩定性測試。結果顯示i-t curve穩定無衰退現象，故GaPt3奈米粒子可做電解水產氫長效型觸媒之應用。
最近，人們一直致力於開發更有活性和穩定的Pd基電催化劑，以部分或完全取代稀有且昂貴的Pt。在這裡，我們開發了一種簡便的熱注射法，並成功合成了分散性佳和形狀控制良好的GaPd2奈米材料，包括多面體、奈米顆粒和奈米線用於HER作為電化學觸媒。所有GaPd2奈米材料都表現出優於商用Pd催化劑的HER活性，並且在酸性介質中顯示其高穩定性。其中，GaPd2納米粒子僅需要24.3 mV的過電位達到10 mA / cm2的電流密度，此效能優於大多數Pt基奈米材料。此外，以伏安法進行10000次CV掃描（−0.3 - 0.2 V vs. RHE）和24小時的穩定性測試，各形狀之GaPd2催化劑都表現出與初始試驗中相近的i-V曲線和穩定的電流密度。我們進一步評估了GaPd2催化劑的質量活性，值得一提的是與商用Pd觸媒相比，GaPd2多面體、奈米顆粒和奈米線在-0.1 V vs. RHE的質量活性方面的表現為商用Pd觸媒的3.7, 5和2.3倍。
MOR和EOR發生於直接醇燃料電池（direct alcohol fuel cell, DAFC）的陽極，所以製備對MOR和EOR具有高度電催化活性的電極觸媒材料對DAFC研究具有重要的意義。我們利用溶液膠體法合成厚度為0.6-0.9 nm的PtSn奈米片作為電氧化觸媒在鹼性和酸性環境中進行MOR和EOR。由於特定的結構和組成特徵， PtSn奈米片相對於商用Pt黑和Pt /碳催化劑皆表現出優異的活性和耐久性。 PtSn奈米片不僅在MOR中表現出優異的質量活性（871.6 mA mg Pt -1），為商用Pt /碳催化劑的2.3倍（371 mA mg Pt -1）和Pt黑的10.1倍（86.1 mA mg Pt -1）; 在EOR也具有673.6 mA mg Pt -1的質量活性，為商用Pt黑（127.7 mA mg Pt -1）的5.3倍，和商用Pt /碳（295 mA mg Pt -1）的2.3倍。和其他以PtSn作為電催化劑的相關研究報導比較，這是MOR和EOR反應中的最佳表現。推測可能原因是由於其小於1 nm的2D片狀形態，導致大量暴露高反應性晶面（111）而造成催化活性提升。

The development of highly active and stable electrocatalysts for the hydrogen evolution reaction (HER) and fuel cell application is one of the main aims to the area of renewable energy. In this study, we describe the synthesis and electrocatalytic applications of noble metal based nanomaterials as electrocatalysts, the main contents are summarized as follows: (1) Popcorn-shaped gallium-platinum (GaPt3) nanoparticles were synthesized and its application as electrocatayst for hydrogen evolution reaction (HER) was investigated (2) Gallium-palladium (GaPd2) were prepared with morphology control for HER application (3) Sub-1nm platinum-tin (PtSn) nanosheets for methanol and ethanol oxidation reactions (MOR and EOR).
In spite of the rapid growth of alternative materials for HER, Pt-based or Pt alloy materials are still the most efficient catalysts. Here, we report a hot-solvent synthesis for producing pop-corn shaped GaPt3 nanoparticles, which exhibits intermetallic behavior with abundant uneven surfaces that guarantee the extensive catalytic active edge sites. The electrochemical catalytic activity of GaPt3-based electrode towards HER was demonstrated for the first time, resulting an outstanding performance of only 27 mV overpotential to achieve the 10 mA/cm2 current density and a Tafel slope of 43.3 mV/dec. (vs. RHE) in acidic media, which is rather superior to that of commercial Pt catalysts and a relatively low overpotential (<80 mV) was obtained even operated at large area (5 cm2). Moreover, cycling tests for 10000-cycle CV sweep (−0.3 to 0.2 V vs. RHE) and durability test for 48 hours were applied and the performance remains still, thus giving the confirmation to the long-lasting feature of GaPt3 nanoparticles.
Recently, great efforts have been focusing on developing more active and stable Pd-based electrocatalyts to partially or completely replace rare and costly Pt. Here we develop a facile hot injection method and successfully synthesis the well-dispersed and shape-controlled GaPd2 nanomaterials including polyhedrons, nanoparticles and nanowires. All the as-synthesized catalysts exhibit superior HER activity than the commercial pure Pd catalyst and stable in the acidic medium. Among them, the GaPd2 nanoparticles required only 24.3 mV overpotential to achieve the 10 mA/cm2 current density, which is outstanding most of the Pt based nanomaterials. Also, cycling tests for 10000-cycle CV sweep (−0.3 to 0.2 vs. RHE) and durability test for 24 hours were applied, the GaPd2 catalysts exhibit similar i-V curves and stable current densities to those obtained in the initial tests. We further evaluate the mass activities of the GaPd2 catalysts, and it is fascinating that the GaPd2 polyhedrons, nanoparticles and nanowires achieved factors of 3.7, 5 and 2.3 enhancement in mass activity at -0.1 V vs. RHE compared with the commercial Pd black catalyst.
Sub-1 nm PtSn nanosheets of 0.6 to 0.9 nm in thickness were syntheiszed via a solution colloidal method and were applied as electrooxidation catalysts MOR and EOR in alkaline and acid environments. Owing to the specific structural and compositional characteristics, the as-prepared PtSn nanosheets exhibits superior activity and durability relative to commercial Pt black and Pt/carbon catalysts. PtSn nanosheets not only exhibit an outstanding mass activity in MOR (871.6 mA mg Pt -1), which is 2.3 times (371 mA mg Pt -1) and 10.1 times (86.1 mA mg Pt -1) higher than that of commercial Pt/carbon and Pt black respectivly, but also display an mass activity in EOR ( 673.6 mA mg Pt -1) with 5.3 times higher commercial Pt black (127.7 mA mg Pt -1) and 2.3 times higher than commercial Pt/C catalyst (295 mA mg Pt -1). The reported value is the highest actitvity in both MOR and EOR exmainations compared to the reported PtSn-based electorcatalysts. The improved performance may be due to the highly-reactive exposed (111) facet sites resulted from its sub-1nm 2D sheet like morphology.

Abstract..............................................................I
中文摘要............................................................III
致謝..................................................................V
Table of Contents....................................................VI
List of Tables.....................................................VIII
List of Figures......................................................IX
Chapter 1. Introduction...............................................1
1 Noble metal nanomaterials.........................................1
2 Hot solvent method................................................2
3 Colloidal method..................................................3
3 Reference.........................................................4
Chapter 2. Synthesis of Popcorn-Shaped Gallium-Platinum (GaPt3) Nanoparticles as Highly Efficient and Stable Electrocatalysts for Hydrogen Evolution Reaction...........................................7
1 Introduction....................................................7
2 Experimental Section............................................9
2.1 Chemicals.......................................................9
2.2 Synthesis of GaPt3 Nanoparticles................................9
2.3 Characterization................................................9
2.4 Electrochemical Measurement....................................10
3 Result and Discussion..........................................11
4 Conclusion.....................................................31
5 Reference......................................................31
Chapter 3. Shape-Controlled Synthesis of Gallium-Palladium (GaPd2) Nanomaterials as High-Performance Electrocatalysts for Hydrogen Evolution Reaction...................................................41
1 Introduction...................................................41
2 Experimental Section...........................................43
2.1 Chemicals......................................................43
2.2 Synthesis of GaPd2 Nanomaterials...............................44
2.3 Characterization...............................................44
2.4 Electrochemical Measurement....................................45
3 Result and Discussion............................................45
4 Conclusion.....................................................60
5 Reference......................................................60
Chapter 4. Sub-1 nm PtSn ultrathin sheet as an extraordinary electrocatalyst for methanol and ethanol oxidation reactions.........68
1 Introduction...................................................68
2 Experimental Section...........................................70
2.1 Chemicals......................................................70
2.2 Synthesis of PtSn nanosheets...................................70
2.3 Characterization...............................................71
2.4 Electrochemical Measurement....................................71
3 Result and Discussion..........................................72
3.1 Synthesis and characterization.................................72
3.2 Methanol Oxidation Reaction (MOR)..............................77
3.3 Ethanol Oxidation Reaction (EOR)...............................81
4 Conclusion.....................................................86
5 Reference......................................................86

                                

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