基于贵金属纳米颗粒/碳纳米材料复合物的燃料电池电催化剂研究
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摘要
燃料电池因其能量转化效率高、污染低、燃料来源广等优点,已成为新能源研究的热点。然而,电催化剂活性较低和价格高昂一直是燃料电池大规模商业化应用的主要障碍。提高催化剂的活性和利用率、降低其用量是目前燃料电池电催化剂研究的重点。为了达到这一目的,通常将小尺寸的贵金属纳米颗粒催化剂均匀分散在具有良好导电性和高比表面积的载体上。
本论文选择碳纳米管和石墨烯为载体,发展了数种载体表面修饰方法,成功实现了贵金属纳米颗粒在这些功能化碳纳米材料表面的小粒径和均匀分布,并系统研究了获得的贵金属纳米颗粒/碳纳米材料复合物对醇类(甲醇、乙醇)、葡萄糖氧化以及氧还原的电催化性能。研究工作主要包括以下几个方面：
(1)以1-烯丙基-3-乙基咪唑四氟硼酸离子液体聚合物修饰的碳纳米管(PIL-CNTs)为载体,银为牺牲模板,通过原位置换法在其表面“生长”具有高分散性和小颗粒尺寸Pt空心球(PtHNs/PIL-CNTs),用循环伏安法、计时电流法考察了PtHNs/PIL-CNTs催化剂在酸性介质中对甲醇的电催化氧化性能。与采用酸氧化碳纳米管通过吸附制备的PtHNs/AO-CNTs和商用E-TEK Pt/C催化剂相比,PtHNs/PIL-CNTs具有高的电催化氧化甲醇质量活性；更重要的是PtHNs/PIL-CNTs电催化氧化甲醇的长期稳定性明显高于其它二种催化剂。
(2)利用氯化钯催化1-甲基-3-炔丙基咪唑溴离子液体聚合制备了炔基离子液体聚合物修饰的碳纳米管(AILP-CNTs),并通过一锅法合成了Pd/AILP-CNTs催化剂。经四探针和交流阻抗研究发现：AILP-CNTs(?)匕1-乙烯-3-乙基咪唑溴离子液体聚合物修饰的碳纳米管具有更好的电子导电性和更小的电荷传递阻力；透射电镜结果表明：平均粒径为3.5±0.5nm的Pd纳米颗粒均匀分布在AILP-CNTs上：循环伏安法、计时电流法研究表明：和基于未功能化处理的碳纳米管制备的Pd/CNTs催化剂相比,Pd/AILP-CNTs在碱性条件下对葡萄糖的电催化氧化具有更高的质量活性和稳定性。
(3)以炔基离子液体聚合物修饰的碳纳米管(AILP-CNTs)为载体,通过硼氢化钠还原制备了PdAu/AILP-CNTs催化剂。透射电镜结果显示：平均粒径为4.5±0.5nm的PdAu纳米颗粒均匀地分散在AILP-CNTs表面；循环伏安法和计时电流法研究发现：与基于未功能化处理的碳纳米管制备的PdAu/CNTs催化剂相比,PdAu/AILP-CNTs在碱性条件下对乙醇的电催化氧化具有更高的活性和电化学稳定性。
(4)用1-芘甲醛(PCA)对碳纳米管进行表面修饰制备了PCA-CNTs,以其为载体,利用PCA的还原性,通过微波辅助还原法制备了PtRu/PCA-CNTs催化剂。透射电镜结果显示：平均粒径为1.7±0.3nm的PtRu纳米颗粒均匀分布在PCA-CNTs表面；循环伏安法和计时电流法研究表明：与以未功能化处理的碳纳米管为载体,通过甲醛还原制备的PtRu/CNTs催化剂相比,PtRu/PCA-CNTs对甲醇的电催化氧化具有更高的活性及长期稳定性。
(5)以1,10-邻二氮杂菲一水合盐酸盐修饰的石墨烯(PNT-GNs)为载体,用微波辅助乙二醇还原的方法制备了Pt/PNT-GNs催化剂。扫描电镜结果显示：Pt纳米颗粒在PNT-GNs表面比在未修饰的石墨烯表面具有更好的分散性和更小的粒径；采用旋转圆盘电极和线性扫描法研究了其对氧还原的电催化性能,结果表明：与基于未修饰石墨烯制备的Pt/GNs催化剂相比,Pt/PNT-GNs具有更好的电催化氧还原活性。
(6)以1-芘甲醛作为石墨烯氧化物(GO)的还原剂,通过还原/功能化一步法制备了羧酸根功能化的、高度还原的石墨烯(PC--GNs),并以其为载体合成了Pt/PC---GNs催化剂。X射线光电子能谱和衍射谱证实了GO的还原,获得的PC—-GNs在水中具有极好的分散性；透射电镜结果显示：平均粒径为1.3+0.2nm的Pt纳米颗粒均匀分布在PC—-GNs表面；循环伏安法和计时电流法研究表明：与基于未修饰石墨烯制备的Pt/GNs催化剂相比,Pt/PC--GNs对甲醇的电催化氧化具有更高的活性及长期稳定性。
Fuel cells have been one of the research hotspots in new energy sources due to high power efficiency, low pollution, abundant sources, and so on. However, the low catalytic activity and high cost of the electrocatalysts are still the key issues hindering the commercial application of fuel cell. At present, the investigation of electrocatalysts focuses on the improvement of the catalytic activity and utilization of the electrocatalysts, and the decrease of the loading mass of noble metals. To achieve this aim, it is desirable that noble metal nanoparticles (NPs) with small size are dispersed uniformly on the supports with good electronic conductivity and high specific surface area.
In this dissertation, several methods for surface modification of carbon supports (carbon nanotubes (CNTs) and graphene) have been developed and noble metal NPs with small particle size have been dispersed uniformly on the functionalized carbon supports. Additionally, the electrocatalytic performances of the obtained noble metal NPs/carbon nanomaterial hybrids towards the oxidation of alcohols (methanol, ethanol), glucose and oxygen reduction have been studied in detail. The main points are summarized as follows:
(1)Taking CNTs modified with poly(1-allyl-3-ethylimidazolium tetrafluoroborate)(PIL-CNTs) as support and silver NPs as sacrified template, Pt hollow nanospheres (PtHNs) with high dispersion and small particle size were successfully "grown" on CNT surface by in-situ displacement method. The electrocatalytic performance of the obtained PtHNs/PIL-CNTs for methanol oxidation in acidic solution was investigated by cyclic voltammetry (CV) and chronoamperometry (CA). Comparing with commercial E-TEK Pt/C and PtHNs adsorbed on acid-oxidized CNTs, PtHNs/PIL-CNTs electrocatalyst has the highest mass activity and best long-term stability for methanol oxidation.
(2) Functionalized CNTs (AILP-CNTs) were prepared by polymerization of1-methyl-3-(prop-2-ynyl)-imidazolium bromide monomers with catalysis of PdCl2, then Pd/AILP-CNTs catalyst was synthesized by one-pot method. The results obtained by the methods of four-point and electrochemical impedance show that AILP-CNTs has better electronic conductivity and smaller charge transfer resistance than CNTs functionalized with poly(1-vinyl-3-ethylimidazolium bromide). Transmission electron microscopy (TEM) result shows that Pd NPs with an average diameter of3.5±0.5nm were uniformly dispersed on the surface of AILP-CNTs. The results from CV and CA demonstrate that Pd/AILP-CNTs catalyst has higher mass activity and stability towards glucose electrooxidation in alkali solution than Pd/CNTs.
(3)With CNTs modified by acetylenic ionic liquid polymer (AILP-CNTs) as support, PdAu/AILP-CNTs electrocatalyst was prepared by NaBH4reduction method. TEM result shows that PdAu NPs with an average diameter of4.5±0.5nm were uniformly dispersed on the surface of AILP-CNTs. The results from CV and CA demonstrate that PdAu/AILP-CNTs catalyst has higher activity and electrochemical stability towards ethanol electrooxidation in alkali solution than PdAu/CNTs.
(4)PCA-CNTs was prepared by the surface modification of CNTs with1-pyrenecarboxaldehyde (PCA). Using the reduction ability of the PCA's aldehyde group, PtRu/PCA-CNTs electrocatalyst was synthesized via microwave-assisted reduction process in water. TEM result shows that Pt NPs with an average diameter of1.7±0.3nm were uniformly dispersed on the surface of PCA-CNTs. The results from CV and CA demonstrate that PtRu/PCA-CNTs catalyst has higher activity and long-term stability towards methanol electrooxidation comparing with PtRu/CNTs catalyst obtained by formaldehyde reduction method.
(5) With1,10-phenanthroline hydrochloride monohydrate-functionalized graphene (PNT-GNs) as support, Pt/PNT-GNs electrocatalyst was prepared by microwave-assisted glycol reduction method. Scanning electron microscopy result shows that Pt NPs on the surface of PNT-GNs had better dispersion and smaller particle size than those on the surface of unmodified graphene. The electrocatalytic performance of Pt/PNT-GNs for oxygen reduction was investigated by rotate disk electrode and linear scanning voltammetry. The results show that Pt/PNT-GNs has better catalytic activity than Pt/GNs.
(6)Using1-pyrenecarboxaldehyde as the reductant for exfoliated graphene oxide (GO), carboxylate-functionalized and high-reduced graphene nanosheets (PC--GNs) were prepared based on a one-step reduction/functionalization strategy. The obtained PC--GNs have excellent dispersibility in water and then are used as support for Pt NPs. Reduction of GO was confirmed by X-ray photoelectron spectroscopy and X-ray diffraction spectroscopy. TEM result shows that Pt NPs with an average diameter of1.3±0.2nm were uniformly dispersed on the surface of PC--GNs. The results from CV and CA demonstrate that Pt/PC--GNs catalyst has higher activity and long-term stability towards methanol electrooxidation comparing with Pt/GNs catalyst.
本论文选择碳纳米管和石墨烯为载体,发展了数种载体表面修饰方法,成功实现了贵金属纳米颗粒在这些功能化碳纳米材料表面的小粒径和均匀分布,并系统研究了获得的贵金属纳米颗粒/碳纳米材料复合物对醇类(甲醇、乙醇)、葡萄糖氧化以及氧还原的电催化性能。研究工作主要包括以下几个方面：
(1)以1-烯丙基-3-乙基咪唑四氟硼酸离子液体聚合物修饰的碳纳米管(PIL-CNTs)为载体,银为牺牲模板,通过原位置换法在其表面“生长”具有高分散性和小颗粒尺寸Pt空心球(PtHNs/PIL-CNTs),用循环伏安法、计时电流法考察了PtHNs/PIL-CNTs催化剂在酸性介质中对甲醇的电催化氧化性能。与采用酸氧化碳纳米管通过吸附制备的PtHNs/AO-CNTs和商用E-TEK Pt/C催化剂相比,PtHNs/PIL-CNTs具有高的电催化氧化甲醇质量活性；更重要的是PtHNs/PIL-CNTs电催化氧化甲醇的长期稳定性明显高于其它二种催化剂。
(2)利用氯化钯催化1-甲基-3-炔丙基咪唑溴离子液体聚合制备了炔基离子液体聚合物修饰的碳纳米管(AILP-CNTs),并通过一锅法合成了Pd/AILP-CNTs催化剂。经四探针和交流阻抗研究发现：AILP-CNTs(?)匕1-乙烯-3-乙基咪唑溴离子液体聚合物修饰的碳纳米管具有更好的电子导电性和更小的电荷传递阻力；透射电镜结果表明：平均粒径为3.5±0.5nm的Pd纳米颗粒均匀分布在AILP-CNTs上：循环伏安法、计时电流法研究表明：和基于未功能化处理的碳纳米管制备的Pd/CNTs催化剂相比,Pd/AILP-CNTs在碱性条件下对葡萄糖的电催化氧化具有更高的质量活性和稳定性。
(3)以炔基离子液体聚合物修饰的碳纳米管(AILP-CNTs)为载体,通过硼氢化钠还原制备了PdAu/AILP-CNTs催化剂。透射电镜结果显示：平均粒径为4.5±0.5nm的PdAu纳米颗粒均匀地分散在AILP-CNTs表面；循环伏安法和计时电流法研究发现：与基于未功能化处理的碳纳米管制备的PdAu/CNTs催化剂相比,PdAu/AILP-CNTs在碱性条件下对乙醇的电催化氧化具有更高的活性和电化学稳定性。
(4)用1-芘甲醛(PCA)对碳纳米管进行表面修饰制备了PCA-CNTs,以其为载体,利用PCA的还原性,通过微波辅助还原法制备了PtRu/PCA-CNTs催化剂。透射电镜结果显示：平均粒径为1.7±0.3nm的PtRu纳米颗粒均匀分布在PCA-CNTs表面；循环伏安法和计时电流法研究表明：与以未功能化处理的碳纳米管为载体,通过甲醛还原制备的PtRu/CNTs催化剂相比,PtRu/PCA-CNTs对甲醇的电催化氧化具有更高的活性及长期稳定性。
(5)以1,10-邻二氮杂菲一水合盐酸盐修饰的石墨烯(PNT-GNs)为载体,用微波辅助乙二醇还原的方法制备了Pt/PNT-GNs催化剂。扫描电镜结果显示：Pt纳米颗粒在PNT-GNs表面比在未修饰的石墨烯表面具有更好的分散性和更小的粒径；采用旋转圆盘电极和线性扫描法研究了其对氧还原的电催化性能,结果表明：与基于未修饰石墨烯制备的Pt/GNs催化剂相比,Pt/PNT-GNs具有更好的电催化氧还原活性。
(6)以1-芘甲醛作为石墨烯氧化物(GO)的还原剂,通过还原/功能化一步法制备了羧酸根功能化的、高度还原的石墨烯(PC--GNs),并以其为载体合成了Pt/PC---GNs催化剂。X射线光电子能谱和衍射谱证实了GO的还原,获得的PC—-GNs在水中具有极好的分散性；透射电镜结果显示：平均粒径为1.3+0.2nm的Pt纳米颗粒均匀分布在PC—-GNs表面；循环伏安法和计时电流法研究表明：与基于未修饰石墨烯制备的Pt/GNs催化剂相比,Pt/PC--GNs对甲醇的电催化氧化具有更高的活性及长期稳定性。
Fuel cells have been one of the research hotspots in new energy sources due to high power efficiency, low pollution, abundant sources, and so on. However, the low catalytic activity and high cost of the electrocatalysts are still the key issues hindering the commercial application of fuel cell. At present, the investigation of electrocatalysts focuses on the improvement of the catalytic activity and utilization of the electrocatalysts, and the decrease of the loading mass of noble metals. To achieve this aim, it is desirable that noble metal nanoparticles (NPs) with small size are dispersed uniformly on the supports with good electronic conductivity and high specific surface area.
In this dissertation, several methods for surface modification of carbon supports (carbon nanotubes (CNTs) and graphene) have been developed and noble metal NPs with small particle size have been dispersed uniformly on the functionalized carbon supports. Additionally, the electrocatalytic performances of the obtained noble metal NPs/carbon nanomaterial hybrids towards the oxidation of alcohols (methanol, ethanol), glucose and oxygen reduction have been studied in detail. The main points are summarized as follows:
(1)Taking CNTs modified with poly(1-allyl-3-ethylimidazolium tetrafluoroborate)(PIL-CNTs) as support and silver NPs as sacrified template, Pt hollow nanospheres (PtHNs) with high dispersion and small particle size were successfully "grown" on CNT surface by in-situ displacement method. The electrocatalytic performance of the obtained PtHNs/PIL-CNTs for methanol oxidation in acidic solution was investigated by cyclic voltammetry (CV) and chronoamperometry (CA). Comparing with commercial E-TEK Pt/C and PtHNs adsorbed on acid-oxidized CNTs, PtHNs/PIL-CNTs electrocatalyst has the highest mass activity and best long-term stability for methanol oxidation.
(2) Functionalized CNTs (AILP-CNTs) were prepared by polymerization of1-methyl-3-(prop-2-ynyl)-imidazolium bromide monomers with catalysis of PdCl2, then Pd/AILP-CNTs catalyst was synthesized by one-pot method. The results obtained by the methods of four-point and electrochemical impedance show that AILP-CNTs has better electronic conductivity and smaller charge transfer resistance than CNTs functionalized with poly(1-vinyl-3-ethylimidazolium bromide). Transmission electron microscopy (TEM) result shows that Pd NPs with an average diameter of3.5±0.5nm were uniformly dispersed on the surface of AILP-CNTs. The results from CV and CA demonstrate that Pd/AILP-CNTs catalyst has higher mass activity and stability towards glucose electrooxidation in alkali solution than Pd/CNTs.
(3)With CNTs modified by acetylenic ionic liquid polymer (AILP-CNTs) as support, PdAu/AILP-CNTs electrocatalyst was prepared by NaBH4reduction method. TEM result shows that PdAu NPs with an average diameter of4.5±0.5nm were uniformly dispersed on the surface of AILP-CNTs. The results from CV and CA demonstrate that PdAu/AILP-CNTs catalyst has higher activity and electrochemical stability towards ethanol electrooxidation in alkali solution than PdAu/CNTs.
(4)PCA-CNTs was prepared by the surface modification of CNTs with1-pyrenecarboxaldehyde (PCA). Using the reduction ability of the PCA's aldehyde group, PtRu/PCA-CNTs electrocatalyst was synthesized via microwave-assisted reduction process in water. TEM result shows that Pt NPs with an average diameter of1.7±0.3nm were uniformly dispersed on the surface of PCA-CNTs. The results from CV and CA demonstrate that PtRu/PCA-CNTs catalyst has higher activity and long-term stability towards methanol electrooxidation comparing with PtRu/CNTs catalyst obtained by formaldehyde reduction method.
(5) With1,10-phenanthroline hydrochloride monohydrate-functionalized graphene (PNT-GNs) as support, Pt/PNT-GNs electrocatalyst was prepared by microwave-assisted glycol reduction method. Scanning electron microscopy result shows that Pt NPs on the surface of PNT-GNs had better dispersion and smaller particle size than those on the surface of unmodified graphene. The electrocatalytic performance of Pt/PNT-GNs for oxygen reduction was investigated by rotate disk electrode and linear scanning voltammetry. The results show that Pt/PNT-GNs has better catalytic activity than Pt/GNs.
(6)Using1-pyrenecarboxaldehyde as the reductant for exfoliated graphene oxide (GO), carboxylate-functionalized and high-reduced graphene nanosheets (PC--GNs) were prepared based on a one-step reduction/functionalization strategy. The obtained PC--GNs have excellent dispersibility in water and then are used as support for Pt NPs. Reduction of GO was confirmed by X-ray photoelectron spectroscopy and X-ray diffraction spectroscopy. TEM result shows that Pt NPs with an average diameter of1.3±0.2nm were uniformly dispersed on the surface of PC--GNs. The results from CV and CA demonstrate that Pt/PC--GNs catalyst has higher activity and long-term stability towards methanol electrooxidation comparing with Pt/GNs catalyst.
引文
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