添加剂对钯纳米晶的形成及电催化性能的影响
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摘要
燃料电池是一种适应未来能源和环境要求的理想电源,目前已经在交通工具、手机电源等行业示范性应用。然而新型燃料电池催化剂铂的昂贵价格是制约其产业化的主要障碍之一,因此,探讨如何降低催化剂的成本、提高催化剂的活性是该领域目前的研究热点。现在较成熟的办法是加入导电的碳材料作为载体,以减少金属的用量,然而碳载体的化学惰性不利于金属的负载,为此要用强酸氧化使其表面官能团化。但是强氧化过程引起的环境污染和对载体表面结构的破坏是其明显的缺点,这促使人们尝试加入有机添加剂,以便改善载体表面化学惰性,使金属催化剂均匀地负载在载体表面,提高催化剂的催化活性和利用率,但是这方面目前还缺乏系统的研究。
本文用钯取代铂作催化剂,以碳纳米管为主要载体,通过加入三类系列变化的添加剂修饰碳载体,以及试用聚吡咯-C60复合载体,分别研究了它们对钯纳米晶的形貌、粒径以及用于甲酸、氢氧化的电催化性能的影响,并探讨了其影响规律。本论文的主要内容有以下几个方面:
一、概述了燃料电池的研究现状、电极催化剂以及催化剂载体的研究进展,阐述了当前燃料电池催化剂研究存在的问题、本文的研究目的及研究内容。
二、选用系列含-OH官能团的添加剂修饰多壁碳纳米管,所选添加剂主要有:HP-β-CD、壳聚糖、乙二醇、邻苯二酚等,分别代表了不同的结构类型。合成了金属钯纳米晶体,研究了添加剂对Pd纳米晶体的形貌、粒径及其对甲酸和氢氧化的电催化性能的影响。结果表明,在所选添加剂的作用下,钯纳米颗粒可以均匀地负载在碳纳米管表面,并且纳米颗粒的粒径和形貌受其结构影响。电催化性能的测试结果表明,在甲酸中活性顺序为:HP-β-CD>邻苯二酚>乙二醇>壳聚糖,在硫酸中活性顺序为:HP-β-CD>邻苯二酚>壳聚糖>乙二醇,我们从分子结构的角度,进一步讨论了这一顺序产生的原因。
三、分别用柠檬酸钠、草酸钠、邻苯二甲酸和海藻酸钠等系列含-COOH官能团添加剂修饰碳纳米管作载体,合成了钯纳米晶体,并研究不同结构添加剂对钯纳米晶的形貌、粒径以及电催化活性的影响。结果表明,在以上几种含-COOH官能团添加剂的作用下,金属钯纳米颗粒分散性较好地负载在碳纳米管表面,并且均有进一步团聚成簇状结构的趋势。钯纳米晶体的粒径有以下顺序:柠檬酸钠≈草酸钠<邻苯二甲酸<海藻酸钠;在硫酸中的活性顺序为:柠檬酸钠>草酸钠>海藻酸钠>邻苯二甲酸;在甲酸中的活性顺序为:草酸钠>柠檬酸钠>海藻酸钠>邻苯二甲;稳定性顺序为:邻苯二甲酸>柠檬酸钠>海藻酸钠>草酸钠。我们讨论了该实验结果与添加剂结构的关系。
四、分别用邻菲啰啉（phen)、聚吡咯(ppy)、聚苯胺(PANI)、乙二胺(en)等系列含N添加剂修饰碳纳米管作载体,合成了高分散性金属钯纳米结构晶体,并研究了不同结构添加剂对纳米晶体的形貌、粒径以及电催化活性的影响。结果表明,以phen或ppy为添加剂时,可以得到高分散金属钯纳米小颗粒,并且催化剂活性明显提高。为了进一步改善催化剂的活性,又以ppy-C为复合载体,以新制备纳米钴颗粒为模板,通过表面置换,在常温下分别合成了Pd/ppy-XC-72和Pd/ppy-MWCNTs纳米空壳结构催化剂,并且对它们的电化学性能进行了表征,结果表明这种空壳结构催化剂对甲酸氧化有很好的电催化性能。
五、分别以ppy、HP-β-CD、柠檬酸钠为添加剂修饰载体C60作为一种新型复合载体,并在载体表面均匀沉积了钯纳米晶体,研究了不同结构添加剂对纳米晶体的形貌、粒径以及电催化活性的影响。结果表明,不同官能团修饰载体C60可以得到不同形貌催化剂:ppy修饰C60时,在载体表面形成粒径均一、高分散的纳米小颗粒;后两种添加剂修饰C60时,则形成由小颗粒组成的纳米簇状结构。不同添加剂作用下金属钯纳米晶粒径大小顺序为:ppyHP-β-CD>柠檬酸钠,即:催化剂Pd/ppy-C60的活性最好,这可能与ppy的导电性和含氮结构有关。
六、对上述研究结果进行归纳总结,探讨了三类不同添加剂和载体对钯纳米晶的形貌、粒径及电催化性能的影响规律。结果表明,含N官能团添加剂修饰载体时有利于金属颗粒的分散性;含-COOH,-OH官能团的添加剂修饰载体时,金属小颗粒容易聚集成纳米簇状结构;小分子添加剂有利于提高催化剂的活性,但是长链大分子或含苯环的添加剂有利于提高催化剂的稳定性。
Fuel cell is a kind of ideal power source to suit for the future energy and environmental requirements, and its prospective application involves clean power generation, transportation,space navigation. However, low oxidation activity of formic acid and high cost of Pt-based catalysts are the major drawbacks to limit the DFAFC’s practical application. Therefore, considerable efforts have been focused on the exploration of less expensive, more abundant non-platinum catalysts with enhanced performance. In the preparation of catalysts on the supports, one of the significant challenges is how to deposit metal nanoparticles uniformly on the surface of them due to their inherent inertness. In order to anchor and deposit catalyst nanoparticles on the surface of the supports, we modified the surface of support, which could increase the electrocatalytic activity and utilization ratio of catalyst.
Pd catalyst was found to possess superior performances in formic acid oxidation compared with Pt-based catalysts. In addition, as the amount of Pd is much more abundant on the earth than that of Pt, it is considered as substitute of Pt for catalyst in DFAFC. Surface modification of carbon supports was carried out by many kinds of additives with different functional groups, such as N element, hydroxyl (–OH), carboxyl (–COOH) groups. Their influence on the catalysts’morphology, partical size and the electrical properties was studied. The main contents of the thesis are following:
Firstly, not only the current research of the fuel cell , the progress of catalyst and catalyst support were given, but also the current questions about the fuel cell catalyst, objective and the main research contents of this paper were described in detail.
Secondly, MWCNTs modified with -OH functional groups of different additives were used as composite supports for synthesizing nanostructured palladium catalysts for formic acid oxidation. The selected additives contain HP-β-CD, Chitosan, Glycol, Catechol and so on. And the influence of the additives on the catalysts’morphology, partical size and the electrical properties was studied. The results suggest that palladium nanoparticles can be deposited on the surface of MWCNTs, and have the trendency to further reunion to cluster-like structures at the presence of the -OH functional groups. The activity order of palladium catalyst in H2SO4 is as follows: HP-β-CD > catechol > Chitosan > ethylene glycol. And the activity for formic acid oxidation is in sequence as follows: HP-β-CD > catechol > ethylene glycol > chitosan. Furthermore, the reason of activity order was discussed from the perspective of the molecular structure.
Thirdly, sodium citrate, sodium oxalate, phthalate and sodium alginate were used as additives to modified MWCNTs, all of which contain -COOH functional groups. Then the formed compositions were used as supports of nanostructured palladium catalysts for formic acid oxidation. The influence of different structured additives on the catalyst morphology, particle size and electrocatalytic activity were studied. The results suggest that on the effect of the -COOH functional groups, palladium nanoparticles can be deposited on the surface of MWCNTs, and have the trendency to further reunion to cluster-like structures. The order of the particle size is as follows: sodium citrate≈sodium oxalate < phthalate < sodium alginate; the activity order: citrate > oxalate > sodium alginate > phthalate; and stability order: phthalate > citrate > sodium alginate > oxalate.
Fourthly, we prepared highly dispersed palladium nanostructured catalyst with MWCNTs as supports, which was modified by the phen, ppy, PANI, en etc, respectively. The influence of the additives on the catalysts’morphology, partical size and the electrical properties was studied. The results showed that the palladium nanoparticles were well-dispersed on the surface of MWCNTs with a relatively narrow particle size distribution at the presence phen or ppy, and the electrocatalytic activity increased significantly. On this basis, to further improve the catalytic activity, we prepared hollow nanospheres catalyst Pd/ppy-XC-72 and Pd/ppy-MWCNTs. In the preparation progress, Co nanoparticles as sacrificial templates were deposited on the prepared polypyrrole-carbon composites by chemical reduction, and then Pd hollow nanospheres formed through the surface replacement reaction between the surface of Co nanoparticles and PdCl2 at room temperature. The catalysts of hollow structure Pd showed a very high electrochemically-active surface area and significant increase in electrocatalytic activity towards formic acid oxidation, which make them the preferable catalysts for direct formic acid fuel cells (DFAFC).
Fifthly, the composite of additive-modified C60 was introduced as a new type of support of nanostructured palladium catalysts for formic acid oxidation. The additives included ppy, HP-β-CD and sodium citrate. The influence of different structured additives on the catalyst morphology, particle size and electrocatalytic activity were studied. The results show that the functionalized C60 composite support can control the particle size and increase dispersivity, and different functional groups can lead to different morphology. The uniform and well-dispersed Pd nanoparticles can be obtained on ppy-modified C60, while the Pd nanocluster catalysts were prepared at the presence of HP-β-CD or sodium citrate. The results were consistent with that with MWCNTs as support. The order of the particle size is as follows: ppy HP-β-CD > sodium citrate. Furthermore, because of the special structure and strong adsorption capacity to metal, the C60 may increase the metal loading. Therefore, the ppy-C60 catalyst may be a kind of more promising catalyst. The electrocatalytic activity of the as-prepared Pd/ppy-C60 catalysts for the oxidation of formic acid is much higher than those of others, showing that the ppy-C60 may be a better potential candidate to be used as the supports of catalyst for electrochemical oxidation.
Sixthly, we summarized the above studies to explore the influence law of different additives and supports on the formation and catalytic properties of the catalysts.
本文用钯取代铂作催化剂,以碳纳米管为主要载体,通过加入三类系列变化的添加剂修饰碳载体,以及试用聚吡咯-C60复合载体,分别研究了它们对钯纳米晶的形貌、粒径以及用于甲酸、氢氧化的电催化性能的影响,并探讨了其影响规律。本论文的主要内容有以下几个方面:
一、概述了燃料电池的研究现状、电极催化剂以及催化剂载体的研究进展,阐述了当前燃料电池催化剂研究存在的问题、本文的研究目的及研究内容。
二、选用系列含-OH官能团的添加剂修饰多壁碳纳米管,所选添加剂主要有:HP-β-CD、壳聚糖、乙二醇、邻苯二酚等,分别代表了不同的结构类型。合成了金属钯纳米晶体,研究了添加剂对Pd纳米晶体的形貌、粒径及其对甲酸和氢氧化的电催化性能的影响。结果表明,在所选添加剂的作用下,钯纳米颗粒可以均匀地负载在碳纳米管表面,并且纳米颗粒的粒径和形貌受其结构影响。电催化性能的测试结果表明,在甲酸中活性顺序为:HP-β-CD>邻苯二酚>乙二醇>壳聚糖,在硫酸中活性顺序为:HP-β-CD>邻苯二酚>壳聚糖>乙二醇,我们从分子结构的角度,进一步讨论了这一顺序产生的原因。
三、分别用柠檬酸钠、草酸钠、邻苯二甲酸和海藻酸钠等系列含-COOH官能团添加剂修饰碳纳米管作载体,合成了钯纳米晶体,并研究不同结构添加剂对钯纳米晶的形貌、粒径以及电催化活性的影响。结果表明,在以上几种含-COOH官能团添加剂的作用下,金属钯纳米颗粒分散性较好地负载在碳纳米管表面,并且均有进一步团聚成簇状结构的趋势。钯纳米晶体的粒径有以下顺序:柠檬酸钠≈草酸钠<邻苯二甲酸<海藻酸钠;在硫酸中的活性顺序为:柠檬酸钠>草酸钠>海藻酸钠>邻苯二甲酸;在甲酸中的活性顺序为:草酸钠>柠檬酸钠>海藻酸钠>邻苯二甲;稳定性顺序为:邻苯二甲酸>柠檬酸钠>海藻酸钠>草酸钠。我们讨论了该实验结果与添加剂结构的关系。
四、分别用邻菲啰啉（phen)、聚吡咯(ppy)、聚苯胺(PANI)、乙二胺(en)等系列含N添加剂修饰碳纳米管作载体,合成了高分散性金属钯纳米结构晶体,并研究了不同结构添加剂对纳米晶体的形貌、粒径以及电催化活性的影响。结果表明,以phen或ppy为添加剂时,可以得到高分散金属钯纳米小颗粒,并且催化剂活性明显提高。为了进一步改善催化剂的活性,又以ppy-C为复合载体,以新制备纳米钴颗粒为模板,通过表面置换,在常温下分别合成了Pd/ppy-XC-72和Pd/ppy-MWCNTs纳米空壳结构催化剂,并且对它们的电化学性能进行了表征,结果表明这种空壳结构催化剂对甲酸氧化有很好的电催化性能。
五、分别以ppy、HP-β-CD、柠檬酸钠为添加剂修饰载体C60作为一种新型复合载体,并在载体表面均匀沉积了钯纳米晶体,研究了不同结构添加剂对纳米晶体的形貌、粒径以及电催化活性的影响。结果表明,不同官能团修饰载体C60可以得到不同形貌催化剂:ppy修饰C60时,在载体表面形成粒径均一、高分散的纳米小颗粒;后两种添加剂修饰C60时,则形成由小颗粒组成的纳米簇状结构。不同添加剂作用下金属钯纳米晶粒径大小顺序为:ppy
六、对上述研究结果进行归纳总结,探讨了三类不同添加剂和载体对钯纳米晶的形貌、粒径及电催化性能的影响规律。结果表明,含N官能团添加剂修饰载体时有利于金属颗粒的分散性;含-COOH,-OH官能团的添加剂修饰载体时,金属小颗粒容易聚集成纳米簇状结构;小分子添加剂有利于提高催化剂的活性,但是长链大分子或含苯环的添加剂有利于提高催化剂的稳定性。
Fuel cell is a kind of ideal power source to suit for the future energy and environmental requirements, and its prospective application involves clean power generation, transportation,space navigation. However, low oxidation activity of formic acid and high cost of Pt-based catalysts are the major drawbacks to limit the DFAFC’s practical application. Therefore, considerable efforts have been focused on the exploration of less expensive, more abundant non-platinum catalysts with enhanced performance. In the preparation of catalysts on the supports, one of the significant challenges is how to deposit metal nanoparticles uniformly on the surface of them due to their inherent inertness. In order to anchor and deposit catalyst nanoparticles on the surface of the supports, we modified the surface of support, which could increase the electrocatalytic activity and utilization ratio of catalyst.
Pd catalyst was found to possess superior performances in formic acid oxidation compared with Pt-based catalysts. In addition, as the amount of Pd is much more abundant on the earth than that of Pt, it is considered as substitute of Pt for catalyst in DFAFC. Surface modification of carbon supports was carried out by many kinds of additives with different functional groups, such as N element, hydroxyl (–OH), carboxyl (–COOH) groups. Their influence on the catalysts’morphology, partical size and the electrical properties was studied. The main contents of the thesis are following:
Firstly, not only the current research of the fuel cell , the progress of catalyst and catalyst support were given, but also the current questions about the fuel cell catalyst, objective and the main research contents of this paper were described in detail.
Secondly, MWCNTs modified with -OH functional groups of different additives were used as composite supports for synthesizing nanostructured palladium catalysts for formic acid oxidation. The selected additives contain HP-β-CD, Chitosan, Glycol, Catechol and so on. And the influence of the additives on the catalysts’morphology, partical size and the electrical properties was studied. The results suggest that palladium nanoparticles can be deposited on the surface of MWCNTs, and have the trendency to further reunion to cluster-like structures at the presence of the -OH functional groups. The activity order of palladium catalyst in H2SO4 is as follows: HP-β-CD > catechol > Chitosan > ethylene glycol. And the activity for formic acid oxidation is in sequence as follows: HP-β-CD > catechol > ethylene glycol > chitosan. Furthermore, the reason of activity order was discussed from the perspective of the molecular structure.
Thirdly, sodium citrate, sodium oxalate, phthalate and sodium alginate were used as additives to modified MWCNTs, all of which contain -COOH functional groups. Then the formed compositions were used as supports of nanostructured palladium catalysts for formic acid oxidation. The influence of different structured additives on the catalyst morphology, particle size and electrocatalytic activity were studied. The results suggest that on the effect of the -COOH functional groups, palladium nanoparticles can be deposited on the surface of MWCNTs, and have the trendency to further reunion to cluster-like structures. The order of the particle size is as follows: sodium citrate≈sodium oxalate < phthalate < sodium alginate; the activity order: citrate > oxalate > sodium alginate > phthalate; and stability order: phthalate > citrate > sodium alginate > oxalate.
Fourthly, we prepared highly dispersed palladium nanostructured catalyst with MWCNTs as supports, which was modified by the phen, ppy, PANI, en etc, respectively. The influence of the additives on the catalysts’morphology, partical size and the electrical properties was studied. The results showed that the palladium nanoparticles were well-dispersed on the surface of MWCNTs with a relatively narrow particle size distribution at the presence phen or ppy, and the electrocatalytic activity increased significantly. On this basis, to further improve the catalytic activity, we prepared hollow nanospheres catalyst Pd/ppy-XC-72 and Pd/ppy-MWCNTs. In the preparation progress, Co nanoparticles as sacrificial templates were deposited on the prepared polypyrrole-carbon composites by chemical reduction, and then Pd hollow nanospheres formed through the surface replacement reaction between the surface of Co nanoparticles and PdCl2 at room temperature. The catalysts of hollow structure Pd showed a very high electrochemically-active surface area and significant increase in electrocatalytic activity towards formic acid oxidation, which make them the preferable catalysts for direct formic acid fuel cells (DFAFC).
Fifthly, the composite of additive-modified C60 was introduced as a new type of support of nanostructured palladium catalysts for formic acid oxidation. The additives included ppy, HP-β-CD and sodium citrate. The influence of different structured additives on the catalyst morphology, particle size and electrocatalytic activity were studied. The results show that the functionalized C60 composite support can control the particle size and increase dispersivity, and different functional groups can lead to different morphology. The uniform and well-dispersed Pd nanoparticles can be obtained on ppy-modified C60, while the Pd nanocluster catalysts were prepared at the presence of HP-β-CD or sodium citrate. The results were consistent with that with MWCNTs as support. The order of the particle size is as follows: ppy
Sixthly, we summarized the above studies to explore the influence law of different additives and supports on the formation and catalytic properties of the catalysts.
引文
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