质子交换膜燃料电池催化剂的研究
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摘要
1839年,格罗夫教授首次提出了燃料电池的概念。二十世纪六十年代,通用电气公司为美国航天局设计开发了质子交换膜燃料电池(PEMFC),当时主要是作为宇宙飞船的能源之用。二十世纪八十年代,加拿大巴拉德公司开始大力开发PEMFC,该领域随即蓬勃发展起来。近年来,由于能源和环境问题逐渐被社会所重视,质子交换膜燃料电池这种清洁而高效的新能源技术也得到了重视和发展。
迄今为止,PEMFC在民用方面仍然没能得到大规模的应用。这关键是由于构成燃料电池的几种关键材料在性能和价格上的缺陷一直难以攻克,导致其应用受限。其中催化剂就是制约燃料电池发展的关键材料之一。
如何制备高活性、长寿命、价格低廉的电催化剂一直是PEMFC催化剂研究的焦点。在催化剂的制备过程中,反应条件会影响所得催化剂的性能。本文通过调变不同的反应条件,系统研究了制备过程中温度、溶液组成、起始pH值、后处理方法等对催化剂形貌,负载情况,稳定性及担载量等性质的影响。
催化剂的载体虽不直接参与电化学反应,但它能够决定活性金属组分的分布状态,而且参与电极中电子的传递和水的传输。载体的物化性质(如比表面积、孔隙分布、导电性、表面官能基团、亲水疏水特性等)会直接影响催化剂的性能。本文选取了具有不同物化性质的碳材料作为催化剂的载体。通过观察所制得催化剂的催化行为,评价了载体的各方面物化性质对催化性能的影响。为催化剂载体材料的选取提供了理论基础。主要研究工作如下:
1.制备了铂纳米颗粒的胶体溶液,并研究了反应条件对铂胶体的影响。同时考察了铂胶体溶液的稳定性。将所得到的铂胶体颗粒在一定的条件下负载到碳载体上,制得了铂担载量为20 wt%的Pt/C催化剂。
2.以乙二醇和甲醛作为还原剂,通过液相还原法制备了Pt/C催化剂,其中Pt颗粒的粒径约为3 nm,分散性良好。此外,还考察了反应时间、反应温度、体系pH值,溶剂组成等条件对催化剂的影响。并发明了一种步骤简单、条件温和的制备燃料电池催化剂的方法,该方法可控性良好。
3.研究了反应后处理方法(洗涤溶剂、干燥条件)对催化剂形貌和性能的影响。发现乙醇淋洗会导致碳载体上的铂颗粒脱落并聚集;加热烘干会导致催化剂碳载体上的铂颗粒脱落、聚集并长大。
4.选取了明胶基碳球、高比表面积活性炭、碳纳米管和Vulcan XC-72等具有不同比表面积、孔隙分布、石墨化程度等物化性能的碳材料作为载体制成Pt/C催化剂,并考察了材料的物化性能对催化剂形貌和催化活性的影响。发现碳纳米管是最理想的催化剂载体材料。
5.选取了具有不同管径的多壁碳纳米管作为载体制备了铂担载量为40 wt%的Pt/C催化剂。并将催化剂制成单电池测试其极化曲线。考察了在不同的工作条件下(温度、氧化剂),载体碳纳米管的管径对催化剂催化活性的影响。发现在低温或者纯氧条件下,管径较大的碳纳米管载铂催化剂具有较好的催化性能,而在高温、空气作氧化剂的条件下,管径为10 ~ 20 nm的碳纳米管载铂催化剂相比于其它催化剂具有最佳催化性能。
6.制备了Pt-Fe/C、Pt-Co/C和Pt-Ni/C几种铂基合金催化剂。并研究了合金催化剂中,铂之外的另一种合金金属对催化剂活性的影响。此外,制备了非铂型Pd/C催化剂,并通过调变反应条件,将Pd颗粒的粒径从几十纳米降至5 ~ 9 nm。
In 1839, Professor Grove first proposed the concept of a fuel cell. Proton exchange membrane fuel cell (PEMFC) was designed by General Electric Company for NASA in the 1960s. At that time, it was only used as the power sources of space craft. PEMFC was blooming since 1980s, when Canadian Ballard began to develop its technology. During the past decade, with environment-protection and energy problems being taken into account, PEMFC as a clean and high effective energy has been paid attention to and developed.
So far, PEMFC in civil applications is still very limit. This is because several key materials of PEMFC too expensive to civil applications. And catalyst is one of the key materials.
The problem how to prepare an electro-catalyst with high activity and long lifetime is one of the key technologies for the PEMFC. The reaction activity of the catalyst can be adjusted by changing the preparing condition. In this paper, the preparation of the catalysts was studied in details on the reacting temperature, the composition of the solution, the pH value of the solution, and the post-processing, which significantly influenced the form and appearance, the loads of Pt, stability and activities of the catalysts.
In addition, the catalyst carrier is not directly involved in electrochemical reaction, but it can determine the distribution of platinum and is involved in electron transfer and water transmission. Physicochemical properties of catalyst carrier (e.g. specific surface area, pore distribution, electrical conductivity, surface functional groups and hydrophilic property) directly affect the activities of the catalyst. In this paper, we chose several carbon materials with different physicochemical properties as the catalyst carriers, and investigated the effects of physicochemical properties of carbon carrier on the activities of the catalyst for proton exchange membrane fuel cell. The main research performance in present dissertation can be summarized and demonstrated as follows:
1. Colloid solution of platinum nanoparticles was prepared. The effect of reacting conditions in the relevance to the properties of platinum colloids was investigated. And the storage stability of platinum colloids was investigated. 20 wt% Pt/C catalyst was prepared by loading platinum nanoparticles on the carbon carrier under certain condition.
2. The Pt/C catalysts were prepared via liquid phase reduction method, using ethylene glycol or formaldehyde as the reducing agent. The diameter of Pt particles was about 3nm. The preparation of the catalysts was studied in details on the reacting time, temperature, the pH value of the solution and the composition of the solution which significantly influenced the activities of the catalysts.
3. The effect of post-processing on the morphology and activities of the catalyst was investigated. The platinum nanoparticles will come off the carrier and aggregate when eluting by ethanol or heating.
4. Low-surface-area gelatin-based porous carbon bead, high-surface-area active carbon, multiwall carbon nanotube and Vulcan carbon XC-72 were chosen to prepare Pt/C catalysts. The effect of physicochemical properties of carbon materials on the morphology and activities of the catalyst was investigated. Carbon nanotube is a promising carrier for PEMFC catalyst.
5. Platinum supported on carbon nanotubes with different tube diameter were prepared. Catalysts were studied by polarization curves. The effect of the tube diameter of carbon nanotubes on the activities of the catalysts was studied under different operating conditions (e.g. operating temperature, oxidant). It was find that at high temperature and air condition, carbon nanotube with its tube diameter of 10 ~ 20 nm support platinum has the best activities.
6. Low platinum catalysts such as Pt-Fe/C, Pt-Co/C and Pt-Ni/C were prepared. The effect of another metal in alloy on the activities of the catalysts was studied. Non-platinum catalysts such as Pd/C were prepared. The diameter of Pd particles was 5 ~ 9 nm.
迄今为止,PEMFC在民用方面仍然没能得到大规模的应用。这关键是由于构成燃料电池的几种关键材料在性能和价格上的缺陷一直难以攻克,导致其应用受限。其中催化剂就是制约燃料电池发展的关键材料之一。
如何制备高活性、长寿命、价格低廉的电催化剂一直是PEMFC催化剂研究的焦点。在催化剂的制备过程中,反应条件会影响所得催化剂的性能。本文通过调变不同的反应条件,系统研究了制备过程中温度、溶液组成、起始pH值、后处理方法等对催化剂形貌,负载情况,稳定性及担载量等性质的影响。
催化剂的载体虽不直接参与电化学反应,但它能够决定活性金属组分的分布状态,而且参与电极中电子的传递和水的传输。载体的物化性质(如比表面积、孔隙分布、导电性、表面官能基团、亲水疏水特性等)会直接影响催化剂的性能。本文选取了具有不同物化性质的碳材料作为催化剂的载体。通过观察所制得催化剂的催化行为,评价了载体的各方面物化性质对催化性能的影响。为催化剂载体材料的选取提供了理论基础。主要研究工作如下:
1.制备了铂纳米颗粒的胶体溶液,并研究了反应条件对铂胶体的影响。同时考察了铂胶体溶液的稳定性。将所得到的铂胶体颗粒在一定的条件下负载到碳载体上,制得了铂担载量为20 wt%的Pt/C催化剂。
2.以乙二醇和甲醛作为还原剂,通过液相还原法制备了Pt/C催化剂,其中Pt颗粒的粒径约为3 nm,分散性良好。此外,还考察了反应时间、反应温度、体系pH值,溶剂组成等条件对催化剂的影响。并发明了一种步骤简单、条件温和的制备燃料电池催化剂的方法,该方法可控性良好。
3.研究了反应后处理方法(洗涤溶剂、干燥条件)对催化剂形貌和性能的影响。发现乙醇淋洗会导致碳载体上的铂颗粒脱落并聚集;加热烘干会导致催化剂碳载体上的铂颗粒脱落、聚集并长大。
4.选取了明胶基碳球、高比表面积活性炭、碳纳米管和Vulcan XC-72等具有不同比表面积、孔隙分布、石墨化程度等物化性能的碳材料作为载体制成Pt/C催化剂,并考察了材料的物化性能对催化剂形貌和催化活性的影响。发现碳纳米管是最理想的催化剂载体材料。
5.选取了具有不同管径的多壁碳纳米管作为载体制备了铂担载量为40 wt%的Pt/C催化剂。并将催化剂制成单电池测试其极化曲线。考察了在不同的工作条件下(温度、氧化剂),载体碳纳米管的管径对催化剂催化活性的影响。发现在低温或者纯氧条件下,管径较大的碳纳米管载铂催化剂具有较好的催化性能,而在高温、空气作氧化剂的条件下,管径为10 ~ 20 nm的碳纳米管载铂催化剂相比于其它催化剂具有最佳催化性能。
6.制备了Pt-Fe/C、Pt-Co/C和Pt-Ni/C几种铂基合金催化剂。并研究了合金催化剂中,铂之外的另一种合金金属对催化剂活性的影响。此外,制备了非铂型Pd/C催化剂,并通过调变反应条件,将Pd颗粒的粒径从几十纳米降至5 ~ 9 nm。
In 1839, Professor Grove first proposed the concept of a fuel cell. Proton exchange membrane fuel cell (PEMFC) was designed by General Electric Company for NASA in the 1960s. At that time, it was only used as the power sources of space craft. PEMFC was blooming since 1980s, when Canadian Ballard began to develop its technology. During the past decade, with environment-protection and energy problems being taken into account, PEMFC as a clean and high effective energy has been paid attention to and developed.
So far, PEMFC in civil applications is still very limit. This is because several key materials of PEMFC too expensive to civil applications. And catalyst is one of the key materials.
The problem how to prepare an electro-catalyst with high activity and long lifetime is one of the key technologies for the PEMFC. The reaction activity of the catalyst can be adjusted by changing the preparing condition. In this paper, the preparation of the catalysts was studied in details on the reacting temperature, the composition of the solution, the pH value of the solution, and the post-processing, which significantly influenced the form and appearance, the loads of Pt, stability and activities of the catalysts.
In addition, the catalyst carrier is not directly involved in electrochemical reaction, but it can determine the distribution of platinum and is involved in electron transfer and water transmission. Physicochemical properties of catalyst carrier (e.g. specific surface area, pore distribution, electrical conductivity, surface functional groups and hydrophilic property) directly affect the activities of the catalyst. In this paper, we chose several carbon materials with different physicochemical properties as the catalyst carriers, and investigated the effects of physicochemical properties of carbon carrier on the activities of the catalyst for proton exchange membrane fuel cell. The main research performance in present dissertation can be summarized and demonstrated as follows:
1. Colloid solution of platinum nanoparticles was prepared. The effect of reacting conditions in the relevance to the properties of platinum colloids was investigated. And the storage stability of platinum colloids was investigated. 20 wt% Pt/C catalyst was prepared by loading platinum nanoparticles on the carbon carrier under certain condition.
2. The Pt/C catalysts were prepared via liquid phase reduction method, using ethylene glycol or formaldehyde as the reducing agent. The diameter of Pt particles was about 3nm. The preparation of the catalysts was studied in details on the reacting time, temperature, the pH value of the solution and the composition of the solution which significantly influenced the activities of the catalysts.
3. The effect of post-processing on the morphology and activities of the catalyst was investigated. The platinum nanoparticles will come off the carrier and aggregate when eluting by ethanol or heating.
4. Low-surface-area gelatin-based porous carbon bead, high-surface-area active carbon, multiwall carbon nanotube and Vulcan carbon XC-72 were chosen to prepare Pt/C catalysts. The effect of physicochemical properties of carbon materials on the morphology and activities of the catalyst was investigated. Carbon nanotube is a promising carrier for PEMFC catalyst.
5. Platinum supported on carbon nanotubes with different tube diameter were prepared. Catalysts were studied by polarization curves. The effect of the tube diameter of carbon nanotubes on the activities of the catalysts was studied under different operating conditions (e.g. operating temperature, oxidant). It was find that at high temperature and air condition, carbon nanotube with its tube diameter of 10 ~ 20 nm support platinum has the best activities.
6. Low platinum catalysts such as Pt-Fe/C, Pt-Co/C and Pt-Ni/C were prepared. The effect of another metal in alloy on the activities of the catalysts was studied. Non-platinum catalysts such as Pd/C were prepared. The diameter of Pd particles was 5 ~ 9 nm.
引文
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