聚合物/碳纳米管及二氧化钛管基复合材料的研究
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摘要
随着纳米技术被应用到材料科学领域中,以纳米复合材料为代表的新材料研究已经成为了二十一世纪世界各国普遍研究的重点。聚合物基纳米复合材料和贵金属电催化剂材料是目前研究的两个热点。聚合物基纳米复合材料的可设计性使其集聚合物与纳米添加相的双重优势,可以生成性能优异的工程材料以及具有新的特殊性能的功能材料。而贵金属电催化剂材料在燃料电池的研究中至关重要,由于贵金属催化剂材料存在成本高、催化效率低等缺点,在很大程度上影响了燃料电池的实用化。因此,最近几年,寻找能降低贵金属用量和提高催化效率的载体材料成为了人们关注的热点。
本文论述了的纳米复合材料的研究及最新进展,并以聚合物/碳纳米管复合材料和二氧化钛纳米管(TiO_2-NTs)基贵金属纳米复合材料为研究重点,制备了聚合物/碳纳米管复合材料、二氧化钛纳米管及以其为载体的贵金属(Pd、Pt)电催化剂复合材料,并研究了它们的性能。主要内容如下:
1.采用原位聚合法成功制备了聚甲基丙烯酸甲酯/碳纳米管、环氧树脂/碳纳米管和聚苯乙烯/碳纳米管三种纳米复合材料,研究了碳纳米管对聚合物基体摩擦磨损性能的影响。结果表明:碳纳米管的引入使得复合材料的摩擦系数和磨损率都有很大的降低,可以有效地增强聚合物基体的摩擦磨损性能,而且存在一个最佳的添加量,添加量过少或过多都达不到最好的增强效果。对于聚甲基丙烯酸甲酯/碳纳米管复合材料而言,1.0wt%的碳纳米管添加量使增强效果达到最佳;而在环氧树脂/碳纳米管和聚苯乙烯/碳纳米管复合材料中,1.5wt%的碳纳米管使摩擦磨损性能达到最好。对于碳纳米管增强聚合物基体摩擦学性能的机理我们也作了一些讨论,可能的原因主要是碳纳米管优异的力学、热学性能以及复合材料独特的结构等。
2.共聚物比单一聚合物在性能和结构上有很大的提高,因此我们采用原位聚合法成功制备了聚甲基丙烯酸甲酯/聚苯乙烯/多壁碳纳米管共聚物纳米复合材料,并研究了其摩擦学性能。结果表明,1.5wt%的多壁碳纳米管添加量使复合材料的摩擦磨损性能达到最佳,复合材料的磨损率从2.3×10~4 mm~3 N~(-1)m~(-1)降低到1.3×10~4 mm~3 N~(-1)m~(-1),降低了43.4%。通过对复合材料内部结构以及显微硬度、摩擦学等试验结果的分析,我们探讨了多壁碳纳米管增强的机理。
3.采用原位化学氧化聚合法制备了聚苯胺/多壁碳纳米管复合材料并研究了其在中性电解液中的电容器性能。结果表明:在1M NaNO_3溶液、-0.2-0.8V扫描范围以及5mAcm~(-2)的电流密度下,聚苯胺/多壁碳纳米管复合材料的电容量达到了328Fg~(-1),明显优于纯聚苯胺的电容量193F~(-1)。我们还通过恒流充放电和阻抗分析测试,研究了复合材料电容器性能提高的原因。多壁碳纳米管提高聚苯胺电容性能的原因可能有以下几个因素:1)多壁碳纳米管的高比表面积可以使其与聚苯胺基体有更好的界面结合。2)聚苯胺/多壁碳纳米管复合材料形成了一个多孔的三维网络状结构,这提供了大的比表面积并使电解液在三维空间里有较好地储存和传输,复合材料也因此就有了更多的法拉第反应活性点从而也拥有了更大的电容值。3)多壁碳纳米管优异的力学性能和电学性能也大大提高了复合材料的结构稳定性同时降低其内部阻抗。另外,循环稳定性测试表明:聚苯胺/多壁碳纳米管复合材料比聚苯胺基体有更好的循环稳定性,在超级电容器材料领域中必将有着广阔的应用前景。
4.为了降低贵金属的用量和提高其催化效率,寻找具有高比表面积和稳定性的载体材料成为了人们研究的热点。我们采用水热合成法制备了锐钛矿型的TiO_2-NTs并以其为载体制备了Pd/TiO_2-NTs、Pt/TiO_2-NTs电催化剂材料。通过对其在水合肼以及甲醇中电催化性能的研究,结果发现这两种材料都有很好的催化性能,其氧化还原峰的峰电位很负和峰电流也都很高。我们认为TiO_2-NTs高的比表面积和出色的稳定性使贵金属的用量降低同时又提高了其催化效率。另外,我们还讨论了水合肼和甲醇的催化机理。这些都表明TiO_2-NTs是一种很理想的燃料电池电催化剂载体材料。
Nanocomposites have been the research focus in the world in 21th century since nanotechnology has been applied in the materials fields. There are two hots including polymer-based nanocomposites and noble metal catalysts nanocomposites. Because the polymer-based nanocomposites have the advantages of all the components, the nanocomposites with excellent and novel properties can be prepared by designing the structure of the nanocomposites. The noble metal electrocatalysts are very important in the research of the fuel cell. However, the application of the fuel cell has been delayed by the high cost and low catalytic efficiency of noble metal electrocatalysts. So the good carrier materials which can low the cost and imporve the catalytic efficiency have recently been paid much attention.
In this paper, we reviewed the latest development in the research of the nanocomposites. With the focus on the polymer/CNTs nanocomposites and the electrocatalysts nanocomposites using TiO_2-NTs as carrier, we have fabricated the polymer/CNTs nanocomposites, TiO_2-NTs, Pd/TiO_2-NTs and Pt/TiO_2-NTs electrocatalysts nanocomposites. The properties of the synthesized nanocomposites have been investigated in details. The main content is the following:
1. The three kinds of polymer/CNTs nanocomposites, including poly(methyl methacrylate)/CNTs, epoxy/CNTs and polystyrene/CNTs, have been produced successfully by means of in-situ polymerization method. The influence of CNTs on the friction and wear properties of the polymer base were investigated in details.
The results showed that the introduction of CNTs greatly lowed the friction coefficient and wear rate of the nanocomposites. The friction and wear properties of the pure polymer were effectively improved. And the best reinforcement impact could be obtained at the right introduction weight of CNTs. For PMMA/CNTs, the introduction of 1.0wt% CNTs can make the best reinforement. For EP/CNTs and PS/CNTs, the best tribological properties of the nanocomposites can be obtained at the introduction of 1.0wt% CNTs.
And the reinforcement mechanisms of CNTs were proposed. The improvements on the tribological properties of polymer/CNTs nanocomposites were mainly attributed to the following factors: 1) super high mechanical and thermal properties of CNTs; 2) the unique structure of the polymer/CNTs nanocomposites.
2. The copolymer have better properties and structure than the single polymer. PMMA/PS/MWNTs copolymer composites have been fabricated successfully by means of in-situ polymerization method.
The introduction of MWNTs improved the friction and wear properties of the copolymer base. The best tribological properties of the copolymer nanocomposites were obtained at the introduction of 1.5wt% MWNTs. The wear rate of the nanocomposites was decreased by 43.4% from 2.3×10~4 mm~3 N~(-1)m~(-1) to 1.3×10~4 mm~3 N~(-1)m~(-1). The mechanisms of the improvements on the tribological properties were discussed by analysising the experimental data of the structure, tribological experiments of the copolymer nanocomposites.
3. PANI/MWNTs have been synthesized successfully by means of in-situ chemical polymerization method. The electrochemical capacitance performance of the composites was investigated in the solution of 1M NaNO_3 by cyclic voltammetry, electrochemical impedance spectroscopy and galvanostatic charge-discharge tests with a three-electrode system. At the current of 5mAcm~(-2), PANI/MWNTs showed the higher specific capacitance values of 328 Fg~(-1) than the pure PANI (193 Fg~(-1)). The main reasons may be attributed to the following factors: 1) The high surface area of MWNTs can help the conjunction between MWNTs and PANI; 2) the well-coated MWNTs of the composites produced a porous three-dimensional network, which might provide a large surface area and allow excellent electrolyte access and storage in three dimensions. Therefore, PANI/MWNTs composites have more available active sites for faradic reaction and larger specific capacitance than pure PANI. 3) The super high mechanical properties of MWNTs can improve the stability of the composites and excellent conductivity of MWNTs can low the resistance of the composites. So PANI/MWNTs composites with good stability have the promising application as the electrochemical capacitors.
4. The carrier materials with high surface and good stabiligy have attracted much attention because they can low the load of noble metals and improve the catalytic efficiency. So the anatase TiO_2-NTs have been synthesized through the hydrothermal process. Pd/TiO_2-NTs and Pt/TiO_2-NTs electrocatalysts have been fabricated by chemical reduction. The catalytic activity of the two electrocatalysts for CH_3OH andN_2H_4 ? H_2O have been investigated in details. The negative voltage and the highcurrent were obtained. The main factors were the high surface and good stabiligy of TiO_2-NTs. The results imply that TiO_2-NTs are good carrier materials of the fuel cell electrocatalysts.
本文论述了的纳米复合材料的研究及最新进展,并以聚合物/碳纳米管复合材料和二氧化钛纳米管(TiO_2-NTs)基贵金属纳米复合材料为研究重点,制备了聚合物/碳纳米管复合材料、二氧化钛纳米管及以其为载体的贵金属(Pd、Pt)电催化剂复合材料,并研究了它们的性能。主要内容如下:
1.采用原位聚合法成功制备了聚甲基丙烯酸甲酯/碳纳米管、环氧树脂/碳纳米管和聚苯乙烯/碳纳米管三种纳米复合材料,研究了碳纳米管对聚合物基体摩擦磨损性能的影响。结果表明:碳纳米管的引入使得复合材料的摩擦系数和磨损率都有很大的降低,可以有效地增强聚合物基体的摩擦磨损性能,而且存在一个最佳的添加量,添加量过少或过多都达不到最好的增强效果。对于聚甲基丙烯酸甲酯/碳纳米管复合材料而言,1.0wt%的碳纳米管添加量使增强效果达到最佳;而在环氧树脂/碳纳米管和聚苯乙烯/碳纳米管复合材料中,1.5wt%的碳纳米管使摩擦磨损性能达到最好。对于碳纳米管增强聚合物基体摩擦学性能的机理我们也作了一些讨论,可能的原因主要是碳纳米管优异的力学、热学性能以及复合材料独特的结构等。
2.共聚物比单一聚合物在性能和结构上有很大的提高,因此我们采用原位聚合法成功制备了聚甲基丙烯酸甲酯/聚苯乙烯/多壁碳纳米管共聚物纳米复合材料,并研究了其摩擦学性能。结果表明,1.5wt%的多壁碳纳米管添加量使复合材料的摩擦磨损性能达到最佳,复合材料的磨损率从2.3×10~4 mm~3 N~(-1)m~(-1)降低到1.3×10~4 mm~3 N~(-1)m~(-1),降低了43.4%。通过对复合材料内部结构以及显微硬度、摩擦学等试验结果的分析,我们探讨了多壁碳纳米管增强的机理。
3.采用原位化学氧化聚合法制备了聚苯胺/多壁碳纳米管复合材料并研究了其在中性电解液中的电容器性能。结果表明:在1M NaNO_3溶液、-0.2-0.8V扫描范围以及5mAcm~(-2)的电流密度下,聚苯胺/多壁碳纳米管复合材料的电容量达到了328Fg~(-1),明显优于纯聚苯胺的电容量193F~(-1)。我们还通过恒流充放电和阻抗分析测试,研究了复合材料电容器性能提高的原因。多壁碳纳米管提高聚苯胺电容性能的原因可能有以下几个因素:1)多壁碳纳米管的高比表面积可以使其与聚苯胺基体有更好的界面结合。2)聚苯胺/多壁碳纳米管复合材料形成了一个多孔的三维网络状结构,这提供了大的比表面积并使电解液在三维空间里有较好地储存和传输,复合材料也因此就有了更多的法拉第反应活性点从而也拥有了更大的电容值。3)多壁碳纳米管优异的力学性能和电学性能也大大提高了复合材料的结构稳定性同时降低其内部阻抗。另外,循环稳定性测试表明:聚苯胺/多壁碳纳米管复合材料比聚苯胺基体有更好的循环稳定性,在超级电容器材料领域中必将有着广阔的应用前景。
4.为了降低贵金属的用量和提高其催化效率,寻找具有高比表面积和稳定性的载体材料成为了人们研究的热点。我们采用水热合成法制备了锐钛矿型的TiO_2-NTs并以其为载体制备了Pd/TiO_2-NTs、Pt/TiO_2-NTs电催化剂材料。通过对其在水合肼以及甲醇中电催化性能的研究,结果发现这两种材料都有很好的催化性能,其氧化还原峰的峰电位很负和峰电流也都很高。我们认为TiO_2-NTs高的比表面积和出色的稳定性使贵金属的用量降低同时又提高了其催化效率。另外,我们还讨论了水合肼和甲醇的催化机理。这些都表明TiO_2-NTs是一种很理想的燃料电池电催化剂载体材料。
Nanocomposites have been the research focus in the world in 21th century since nanotechnology has been applied in the materials fields. There are two hots including polymer-based nanocomposites and noble metal catalysts nanocomposites. Because the polymer-based nanocomposites have the advantages of all the components, the nanocomposites with excellent and novel properties can be prepared by designing the structure of the nanocomposites. The noble metal electrocatalysts are very important in the research of the fuel cell. However, the application of the fuel cell has been delayed by the high cost and low catalytic efficiency of noble metal electrocatalysts. So the good carrier materials which can low the cost and imporve the catalytic efficiency have recently been paid much attention.
In this paper, we reviewed the latest development in the research of the nanocomposites. With the focus on the polymer/CNTs nanocomposites and the electrocatalysts nanocomposites using TiO_2-NTs as carrier, we have fabricated the polymer/CNTs nanocomposites, TiO_2-NTs, Pd/TiO_2-NTs and Pt/TiO_2-NTs electrocatalysts nanocomposites. The properties of the synthesized nanocomposites have been investigated in details. The main content is the following:
1. The three kinds of polymer/CNTs nanocomposites, including poly(methyl methacrylate)/CNTs, epoxy/CNTs and polystyrene/CNTs, have been produced successfully by means of in-situ polymerization method. The influence of CNTs on the friction and wear properties of the polymer base were investigated in details.
The results showed that the introduction of CNTs greatly lowed the friction coefficient and wear rate of the nanocomposites. The friction and wear properties of the pure polymer were effectively improved. And the best reinforcement impact could be obtained at the right introduction weight of CNTs. For PMMA/CNTs, the introduction of 1.0wt% CNTs can make the best reinforement. For EP/CNTs and PS/CNTs, the best tribological properties of the nanocomposites can be obtained at the introduction of 1.0wt% CNTs.
And the reinforcement mechanisms of CNTs were proposed. The improvements on the tribological properties of polymer/CNTs nanocomposites were mainly attributed to the following factors: 1) super high mechanical and thermal properties of CNTs; 2) the unique structure of the polymer/CNTs nanocomposites.
2. The copolymer have better properties and structure than the single polymer. PMMA/PS/MWNTs copolymer composites have been fabricated successfully by means of in-situ polymerization method.
The introduction of MWNTs improved the friction and wear properties of the copolymer base. The best tribological properties of the copolymer nanocomposites were obtained at the introduction of 1.5wt% MWNTs. The wear rate of the nanocomposites was decreased by 43.4% from 2.3×10~4 mm~3 N~(-1)m~(-1) to 1.3×10~4 mm~3 N~(-1)m~(-1). The mechanisms of the improvements on the tribological properties were discussed by analysising the experimental data of the structure, tribological experiments of the copolymer nanocomposites.
3. PANI/MWNTs have been synthesized successfully by means of in-situ chemical polymerization method. The electrochemical capacitance performance of the composites was investigated in the solution of 1M NaNO_3 by cyclic voltammetry, electrochemical impedance spectroscopy and galvanostatic charge-discharge tests with a three-electrode system. At the current of 5mAcm~(-2), PANI/MWNTs showed the higher specific capacitance values of 328 Fg~(-1) than the pure PANI (193 Fg~(-1)). The main reasons may be attributed to the following factors: 1) The high surface area of MWNTs can help the conjunction between MWNTs and PANI; 2) the well-coated MWNTs of the composites produced a porous three-dimensional network, which might provide a large surface area and allow excellent electrolyte access and storage in three dimensions. Therefore, PANI/MWNTs composites have more available active sites for faradic reaction and larger specific capacitance than pure PANI. 3) The super high mechanical properties of MWNTs can improve the stability of the composites and excellent conductivity of MWNTs can low the resistance of the composites. So PANI/MWNTs composites with good stability have the promising application as the electrochemical capacitors.
4. The carrier materials with high surface and good stabiligy have attracted much attention because they can low the load of noble metals and improve the catalytic efficiency. So the anatase TiO_2-NTs have been synthesized through the hydrothermal process. Pd/TiO_2-NTs and Pt/TiO_2-NTs electrocatalysts have been fabricated by chemical reduction. The catalytic activity of the two electrocatalysts for CH_3OH andN_2H_4 ? H_2O have been investigated in details. The negative voltage and the highcurrent were obtained. The main factors were the high surface and good stabiligy of TiO_2-NTs. The results imply that TiO_2-NTs are good carrier materials of the fuel cell electrocatalysts.
引文
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