低碳醇在钯纳米修饰氧化铟锡电极上的电催化氧化研究
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摘要
直接醇类燃料电池(Direct alcohol fuel cell,缩写为DAFC)作为一种新型的绿色能源,对解决目前世界面临的能源短缺和环境污染这两大难题具有跨时代的重要意义。ITO导电膜玻璃是一种新颖的电极材料,具有良好的导电性和超大的表面积,它可以作为贵金属纳米材料的载体,极大提高催化剂的利用率。基于钯纳米粒子高吸附性、高比表面积、高电催化活性等特点,本论文主要通过循环扫描法制备出高电活性、高灵敏度的钯纳米修饰氧化铟锡(Pd NPs/ITO)电极,并将其应用于低碳醇(包括甲醇、乙醇、丙醇等)的电催化氧化研究中。
第一章:简介直接醇类燃料电池的发展状况,对钯纳米修饰电极在醇电催化氧化中的研究进展进行综述。
第二章:通过化学沉积法和循环伏安扫描法成功制备了Pd NPs/ITO电极。采用循环伏安法考察了标准氧化还原电对[Fe(CN)_6]~(4-)/[Fe(CN)_6]~(3-)中该电极的电活性,并利用电子扫描电镜对电极表面的形貌进行表征。此外还分析研究了电极在不同电势范围内发生的电化学反应过程以及反应温度、通氮气和电极放置时间对电化学检测的影响。结果表明:ITO导电膜玻璃的引入大大提高了电催化剂Pd纳米的利用率,使得Pd NPs/ITO电极具有良好的电活性;由不同电势范围内该电极在碱性溶液中的循环伏安行为可知,对于氢的吸附和脱附可以通过扫描电势范围的大小来控制;经过实验条件的考察得出Pd NPs/ITO电极的最佳反应温度为65℃,电解液中通入氮气可以排除溶解氧的干扰,该电极在1个月内能够保持良好的活性。
第三章:采用简单的循环伏安扫描法制备得到高电活性的Pd NPs/ITO电极,并用该电极研究了室温下氢氧化钠溶液中甲醇和乙醇的电氧化反应,对各自的电化学反应过程进行了详细探讨。随后考察了反应物浓度,扫描速率对甲醇和乙醇在PdNPs/ITO电极上电催化氧化反应的影响。对比发现,甲醇和乙醇在Pd NPs/ITO电极上的电催化活性都比纯金属钯电极好(甲醇约为纯金属钯电极的2倍,乙醇约为纯金属钯电极的4倍)。甲醇和乙醇氧化峰电流的强度均与各自的浓度及扫描速率的开方成正比,且保持良好的线性关系,说明两种醇在Pd NPs/ITO电极上的反应都属于扩散控制过程。
第四章:首先利用循环伏安扫描法制得的Pd NPs/ITO电极研究了室温下碱性电解液中正丙醇和异丙醇的电催化氧化反应,并就反应物浓度,扫描速率对丙醇和异丙醇在该电极上电催化氧化反应的影响进行考察,发现正丙醇和异丙醇氧化峰电流的强度i_(pa)均与各自的浓度c及扫描速率的开方v~(1/2)成正比,说明这两种醇在Pd NPs/ITO电极上的反应都属于扩散控制过程。然后对甲醇、乙醇、正丙醇和异丙醇进行综合对比,得出碱性介质中低碳醇在PdNPs/ITO电极上的电催化氧化符合以下规律:(1)不同醇分子的电氧化具有类似的循环伏安特性。醇的氧化峰电流强度远大于氢的脱附和吸附峰,说明在-1.4～0.6V电势范围内这些醇或其解离产物会吸附在Pd NPs/ITO电极表面并抑制氢的吸附和脱附,使得醇的氧化作用占主导地位;氢的脱附和吸附峰位置相对稳定,分别出现在-0.4V和-0.5V左右;阴极扫描过程中-0.4～0.3V电势范围内的曲线几乎完全重合。(2)根据醇氧化峰电流强度的大小推断出Pd NPs/ITO电极对四种醇的催化活性顺序为:乙醇＞正丙醇＞甲醇＞异丙醇。(3)可以根据醇氧化峰位置的差异大致判断醇的种类。
第五章:利用化学沉积法制备的Pd NPs/ITO电极,通过电化学方法分别在酸性和碱性电解液中初步研究了室温下钯纳米对甲烷气体的电催化响应。发现酸性和碱性电解液中的循环伏安特征相近,只是峰电位不同。通甲烷至饱和后,氧化峰电流强度有所下降,且出现分岔现象,氧化峰位置也向正偏移。可能是由于溶解到电解液中的甲烷部分吸附在PdNPs/ITO电极表面,阻碍了Pd本身的电化学反应,同时经钯纳米催化甲烷的电氧化。这为研制新型甲烷纳米气体传感器提供了新思路。
Direct alcohol fuel cell (Direct alcohol fuel cell, abbreviated as DAFC) as a new type of green energy, has cross-age significance to solve the two current world problems of energy shortage and environmental pollution. Indium-tin oxide (ITO) conductive film glass is a novel electrode material which has good conductivity and large surface area. It can be used as the carrier of noble metal nanomaterials to greatly improve the utilization ratio of catalyst. Based on the properties of palladium nanoparticles with high adsorption ability, high specific surface area and high electrocatalytic activity etc., this paper prepared the palladium nanoparticle-modified indium-tin oxide (Pd NPs/ITO) electrode by cyclic scanning. The electrode has high electrical activity and high sensitivity, which will be applied to study of low-carbon alcohols (including methanol, ethanol, propanol, etc.) for electrocatalytic oxidation.
ChapterⅠ: Development of DAFC was briefly introduced and the development of palladium nanoparticle-modified electrode in electrocatalytic oxidation of alcohols was reviewed.
ChapterⅡ: The Pd NPs/ITO electrode was successfully prepared by chemical deposition method and cyclic voltammetry scanning method. The electrochemical activity of the electrode was studied by cyclic voltammetry using the standard redox of [Fe (CN) _6]~(4-)/ [Fe (CN)_6]~(3-) and the morphology of the electrode surface were characterized by electronic scanning microscopy. In addition, the electrochemical reaction process of the electrode in different scope of potential was analyzed, so did the reaction temperature, effect of nitrogen and placed time for electrodes to the electrochemical detection. The results showed that the utilization ratio of nano-Pd catalyst was greatly improved and had good electrochemical activity due to the introduction of ITO conductive film glass. From the cyclic voltammetry behavior of the electrode in different electric potential range in alkaline solution, it can be obtained that the adsorption and desorption of hydrogen could controlled by the size of scanning electric potential scope. From the study of our experiment, it could be concluded that the best reaction temperature of Pd NPs / ITO electrode was 65℃and interference from dissolved oxygen can be excluded by passing nitrogen through electrolyte. The prepared electrode maintained good activity in a month.
ChapterⅢ: Pd NPs/ITO electrode with high electrical activity has been prepared using a simple cyclic voltammetry scanning method. Then it was used to study the electro-oxidation reaction of methanol and ethanol in sodium hydroxide solution at room temperature and the process of their electrochemical reaction was discussed in detail, respectively. Next, the effect of reactant concentration and scan rate on methanol and ethanol electrocatalytic oxidation reaction on the Pd NPs/ITO electrode was investigated. For comparison, it was found that the electrocatalytic activity of both methanol and ethanol on the Pd NPs/ITO electrode was better than the pure metal palladium electrode (the activity of methanol is about 2 times of pure metal palladium electrode and that of ethanol is about 4 times). The intensity of the oxidation peak current of methanol and ethanol was proportional to their own concentration and extraction of scan rate, and maintained a good linear relationship, which showed that the reaction of two alcohols on the Pd NPs/ITO electrode were diffusion-controlled process.
ChapterⅣ: At first, the Pd NPs/ITO electrode was prepared using cyclic voltammetry. Then it was used to study the electrocatalytic oxidation reaction of n-propanol and isopropanol in alkaline electrolyte at room temperature and effect of reactant concentration and scan rate on the reaction was also studied. It was found that the intensity oxidation peak current i_(pa) of n-propanol and isopropanol alcohol was proportional to their own concentration c and scan rate v~(1/2) , which indicated that the reaction of two alcohols on the Pd NPs/ITO electrode were diffusion-controlled process. And then comprehensive comparison was made among methanol, ethanol, propanol and isopropanol and some conclusions on the electrocatalytic oxidation of lower alcohols in alkaline medium on the Pd NPs/ITO electrode were drawn as follows. (1) There were similar characteristics in cyclic voltammetry among different alcohols. The intensity of oxidation peak of alcohol was far greater than that of hydrogen desorption and absorption, which indicated that these potential alcohol or its dissociation products would be adsorbed on the surface of Pd NPs/ITO electrode in the range of -1.4 ~ 0.6V and simultaneously inhibit the adsorption and desorption of hydrogen leading to the dominant oxidation of alcohol. The peak positions of hydrogen desorption and absorption were relatively stable at about -0.4V and -0.5V, respectively. The curve of cathode scanning within the scope of -0.4 ~ 0.3V was almost completely overlapped. (2) According to the peak current intensity of alcohols on Pd NPs/ITO electrode, the catalytic activity order of four types of alcohols were as following: ethanol> propanol > methanol > isopropanol. (3) According to the difference position of oxidation peak, the type of alcohol could be determined.
ChapterⅤ: Pd NPs / ITO electrode was prepared by chemical deposition. The electrocatalytic response of palladium nanoparticles to methane in acidic and alkaline electrolyte was preliminarily studied through electrochemical method at room temperature, respectively. It was found that cyclic voltammetry characteristics were similar in acidic and alkaline electrolyte, but there was difference in peak potential. Bubbling methane to its saturation in solution, the oxidation peak current intensity has decreased, and the phenomenon of bifurcation appeared, and the oxidation peak shift to the position. It was possibly that methane dissolution in electrolyte partly adsorbed on the surface of Pd NPs/ITO electrode and hindered the electrochemical reaction of Pd itself At the same time, methane was electrooxidized by palladium nanoparticles as catalyst. It was beneficial to the development of novelmethane gas sensors based on nanoparticles.
第一章:简介直接醇类燃料电池的发展状况,对钯纳米修饰电极在醇电催化氧化中的研究进展进行综述。
第二章:通过化学沉积法和循环伏安扫描法成功制备了Pd NPs/ITO电极。采用循环伏安法考察了标准氧化还原电对[Fe(CN)_6]~(4-)/[Fe(CN)_6]~(3-)中该电极的电活性,并利用电子扫描电镜对电极表面的形貌进行表征。此外还分析研究了电极在不同电势范围内发生的电化学反应过程以及反应温度、通氮气和电极放置时间对电化学检测的影响。结果表明:ITO导电膜玻璃的引入大大提高了电催化剂Pd纳米的利用率,使得Pd NPs/ITO电极具有良好的电活性;由不同电势范围内该电极在碱性溶液中的循环伏安行为可知,对于氢的吸附和脱附可以通过扫描电势范围的大小来控制;经过实验条件的考察得出Pd NPs/ITO电极的最佳反应温度为65℃,电解液中通入氮气可以排除溶解氧的干扰,该电极在1个月内能够保持良好的活性。
第三章:采用简单的循环伏安扫描法制备得到高电活性的Pd NPs/ITO电极,并用该电极研究了室温下氢氧化钠溶液中甲醇和乙醇的电氧化反应,对各自的电化学反应过程进行了详细探讨。随后考察了反应物浓度,扫描速率对甲醇和乙醇在PdNPs/ITO电极上电催化氧化反应的影响。对比发现,甲醇和乙醇在Pd NPs/ITO电极上的电催化活性都比纯金属钯电极好(甲醇约为纯金属钯电极的2倍,乙醇约为纯金属钯电极的4倍)。甲醇和乙醇氧化峰电流的强度均与各自的浓度及扫描速率的开方成正比,且保持良好的线性关系,说明两种醇在Pd NPs/ITO电极上的反应都属于扩散控制过程。
第四章:首先利用循环伏安扫描法制得的Pd NPs/ITO电极研究了室温下碱性电解液中正丙醇和异丙醇的电催化氧化反应,并就反应物浓度,扫描速率对丙醇和异丙醇在该电极上电催化氧化反应的影响进行考察,发现正丙醇和异丙醇氧化峰电流的强度i_(pa)均与各自的浓度c及扫描速率的开方v~(1/2)成正比,说明这两种醇在Pd NPs/ITO电极上的反应都属于扩散控制过程。然后对甲醇、乙醇、正丙醇和异丙醇进行综合对比,得出碱性介质中低碳醇在PdNPs/ITO电极上的电催化氧化符合以下规律:(1)不同醇分子的电氧化具有类似的循环伏安特性。醇的氧化峰电流强度远大于氢的脱附和吸附峰,说明在-1.4～0.6V电势范围内这些醇或其解离产物会吸附在Pd NPs/ITO电极表面并抑制氢的吸附和脱附,使得醇的氧化作用占主导地位;氢的脱附和吸附峰位置相对稳定,分别出现在-0.4V和-0.5V左右;阴极扫描过程中-0.4～0.3V电势范围内的曲线几乎完全重合。(2)根据醇氧化峰电流强度的大小推断出Pd NPs/ITO电极对四种醇的催化活性顺序为:乙醇＞正丙醇＞甲醇＞异丙醇。(3)可以根据醇氧化峰位置的差异大致判断醇的种类。
第五章:利用化学沉积法制备的Pd NPs/ITO电极,通过电化学方法分别在酸性和碱性电解液中初步研究了室温下钯纳米对甲烷气体的电催化响应。发现酸性和碱性电解液中的循环伏安特征相近,只是峰电位不同。通甲烷至饱和后,氧化峰电流强度有所下降,且出现分岔现象,氧化峰位置也向正偏移。可能是由于溶解到电解液中的甲烷部分吸附在PdNPs/ITO电极表面,阻碍了Pd本身的电化学反应,同时经钯纳米催化甲烷的电氧化。这为研制新型甲烷纳米气体传感器提供了新思路。
Direct alcohol fuel cell (Direct alcohol fuel cell, abbreviated as DAFC) as a new type of green energy, has cross-age significance to solve the two current world problems of energy shortage and environmental pollution. Indium-tin oxide (ITO) conductive film glass is a novel electrode material which has good conductivity and large surface area. It can be used as the carrier of noble metal nanomaterials to greatly improve the utilization ratio of catalyst. Based on the properties of palladium nanoparticles with high adsorption ability, high specific surface area and high electrocatalytic activity etc., this paper prepared the palladium nanoparticle-modified indium-tin oxide (Pd NPs/ITO) electrode by cyclic scanning. The electrode has high electrical activity and high sensitivity, which will be applied to study of low-carbon alcohols (including methanol, ethanol, propanol, etc.) for electrocatalytic oxidation.
ChapterⅠ: Development of DAFC was briefly introduced and the development of palladium nanoparticle-modified electrode in electrocatalytic oxidation of alcohols was reviewed.
ChapterⅡ: The Pd NPs/ITO electrode was successfully prepared by chemical deposition method and cyclic voltammetry scanning method. The electrochemical activity of the electrode was studied by cyclic voltammetry using the standard redox of [Fe (CN) _6]~(4-)/ [Fe (CN)_6]~(3-) and the morphology of the electrode surface were characterized by electronic scanning microscopy. In addition, the electrochemical reaction process of the electrode in different scope of potential was analyzed, so did the reaction temperature, effect of nitrogen and placed time for electrodes to the electrochemical detection. The results showed that the utilization ratio of nano-Pd catalyst was greatly improved and had good electrochemical activity due to the introduction of ITO conductive film glass. From the cyclic voltammetry behavior of the electrode in different electric potential range in alkaline solution, it can be obtained that the adsorption and desorption of hydrogen could controlled by the size of scanning electric potential scope. From the study of our experiment, it could be concluded that the best reaction temperature of Pd NPs / ITO electrode was 65℃and interference from dissolved oxygen can be excluded by passing nitrogen through electrolyte. The prepared electrode maintained good activity in a month.
ChapterⅢ: Pd NPs/ITO electrode with high electrical activity has been prepared using a simple cyclic voltammetry scanning method. Then it was used to study the electro-oxidation reaction of methanol and ethanol in sodium hydroxide solution at room temperature and the process of their electrochemical reaction was discussed in detail, respectively. Next, the effect of reactant concentration and scan rate on methanol and ethanol electrocatalytic oxidation reaction on the Pd NPs/ITO electrode was investigated. For comparison, it was found that the electrocatalytic activity of both methanol and ethanol on the Pd NPs/ITO electrode was better than the pure metal palladium electrode (the activity of methanol is about 2 times of pure metal palladium electrode and that of ethanol is about 4 times). The intensity of the oxidation peak current of methanol and ethanol was proportional to their own concentration and extraction of scan rate, and maintained a good linear relationship, which showed that the reaction of two alcohols on the Pd NPs/ITO electrode were diffusion-controlled process.
ChapterⅣ: At first, the Pd NPs/ITO electrode was prepared using cyclic voltammetry. Then it was used to study the electrocatalytic oxidation reaction of n-propanol and isopropanol in alkaline electrolyte at room temperature and effect of reactant concentration and scan rate on the reaction was also studied. It was found that the intensity oxidation peak current i_(pa) of n-propanol and isopropanol alcohol was proportional to their own concentration c and scan rate v~(1/2) , which indicated that the reaction of two alcohols on the Pd NPs/ITO electrode were diffusion-controlled process. And then comprehensive comparison was made among methanol, ethanol, propanol and isopropanol and some conclusions on the electrocatalytic oxidation of lower alcohols in alkaline medium on the Pd NPs/ITO electrode were drawn as follows. (1) There were similar characteristics in cyclic voltammetry among different alcohols. The intensity of oxidation peak of alcohol was far greater than that of hydrogen desorption and absorption, which indicated that these potential alcohol or its dissociation products would be adsorbed on the surface of Pd NPs/ITO electrode in the range of -1.4 ~ 0.6V and simultaneously inhibit the adsorption and desorption of hydrogen leading to the dominant oxidation of alcohol. The peak positions of hydrogen desorption and absorption were relatively stable at about -0.4V and -0.5V, respectively. The curve of cathode scanning within the scope of -0.4 ~ 0.3V was almost completely overlapped. (2) According to the peak current intensity of alcohols on Pd NPs/ITO electrode, the catalytic activity order of four types of alcohols were as following: ethanol> propanol > methanol > isopropanol. (3) According to the difference position of oxidation peak, the type of alcohol could be determined.
ChapterⅤ: Pd NPs / ITO electrode was prepared by chemical deposition. The electrocatalytic response of palladium nanoparticles to methane in acidic and alkaline electrolyte was preliminarily studied through electrochemical method at room temperature, respectively. It was found that cyclic voltammetry characteristics were similar in acidic and alkaline electrolyte, but there was difference in peak potential. Bubbling methane to its saturation in solution, the oxidation peak current intensity has decreased, and the phenomenon of bifurcation appeared, and the oxidation peak shift to the position. It was possibly that methane dissolution in electrolyte partly adsorbed on the surface of Pd NPs/ITO electrode and hindered the electrochemical reaction of Pd itself At the same time, methane was electrooxidized by palladium nanoparticles as catalyst. It was beneficial to the development of novelmethane gas sensors based on nanoparticles.
引文
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