导电聚合物/贵金属复合材料的制备及其应用于有机小分子的电催化氧化
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摘要
低温燃料电池作为一种新型的能源装置,具有能量转换效率高、工作温度低、无污染、液体燃料处理简单、启动迅速等诸多优点,已成为世界各国竞相研究的热点。有机小分子的高效电催化氧化直接关系到低温燃料电池的发展和应用。低温燃料电池的电极材料主要是碳/贵金属复合材料,碳载体易导致贵金属粒子团聚、且易发生电氧化腐蚀等缺点降低了贵金属的利用率和电池的使用寿命。导电聚合物/贵金属复合材料具有高的抗腐蚀性、电子/质子双重导电性和协同作用,目前其应用于有机小分子的电催化氧化主要集中于聚苯胺、聚吡咯和聚噻吩及其衍生物与贵金属复合材料的研究。电化学方法是制备导电聚合物/贵金属复合材料的方法之一。随着导电聚合物的发展,许多性能优良的导电聚合物相继出现。本论文利用电化学方法制备一系列新型导电聚合物/贵金属复合材料(聚吲哚及其衍生物/铂、聚咔唑/铂-钌、聚对苯/钯-金等复合材料),以其对有机小分子(甲酸、甲醇和异丙醇等)的电催化氧化活性进行评价,同时,探讨了导电聚合物与贵金属纳米粒子之间的协同作用和影响因素。本文还研究了吲哚小分子修饰铂催化剂对甲酸的高效电催化氧化。结果简述如下:
1.在三氟化硼乙醚及其混合电解质中分别电化学制备聚吲哚、聚(5-甲氧基吲哚)、聚(5-硝基吲哚)、聚(5-氰基吲哚)等导电聚合物,首次以这些聚合物作为铂催化剂载体。制备的聚吲哚衍生物/铂复合材料通过SEM、XRD及其电化学方法进行了表征。相比于传统的聚吡咯/铂复合催化剂,所制备的四种聚吲哚/铂复合催化剂对甲酸具有更高的电催化活性和和抗毒化能力。这种提高的效果主要来自于聚吲哚及其衍生物与铂之间的协同作用和铂的电化学活性位点的增加,这种协调作用促进了甲酸的直接电化学氧化。另一方面,相比于聚吡咯/铂复合催化剂,聚吲哚/Pt和聚(5-甲氧基吲哚)/Pt复合材料对甲醇具有更高的电催化氧化能力和抗毒化能力。
2.在三氟化硼乙醚+ 50%乙醚混合电解质中电化学制备了聚咔唑,首次以聚咔唑为载体负载铂、铂-钌双金属催化剂,详细研究了酸性介质中聚咔唑/铂、聚咔唑/铂-钌复合催化剂对甲酸和甲醇的电化学氧化。聚咔唑在0.5M H2SO4溶液中具有很好的导电性和电化学活性。制备的复合材料通过SEM、EDS和电化学方法进行了表征。相比于电沉积在裸玻碳电极上的铂-钌双金属催化剂,聚咔唑/铂和聚咔唑/铂-钌复合催化剂对甲醇的电化学氧化的促进效果较弱,然而,聚咔唑/铂和聚咔唑/铂-钌复合催化剂对甲酸具有更高的电催化活性和稳定性。这种促进效果可能来自于金属与聚咔唑之间的协同作用。CO的剥离实验结果表明,CO在聚咔唑/铂和聚咔唑/铂-钌复合催化剂上的吸附强度大大减弱、且CO更容易氧化去除。
3.我们发现聚(5-硝基吲哚)在碱性溶液中具有良好的电化学活性和稳定性,因此,我们首次研究了聚(5-硝基吲哚)负载铂催化剂在碱性介质中对甲醇的电化学氧化。详细考察了不同参数对甲醇的电催化氧化的影响,例如:膜的量、铂的载量、KOH和甲醇的浓度、扫描速率和不同的碱性电解质等等。相比于电沉积在裸玻碳电极上的铂催化剂,所制备的聚(5-硝基吲哚)/铂复合催化剂在碱性下对甲醇具有更高的电催化活性和稳定性。
4.在纯三氟化硼乙醚电解质中,以联苯为单体低电位电化学制备了聚对苯,首次以聚对苯为载体成功地负载钯-金双金属催化剂,分别详细研究了聚对苯/钯-金复合催化剂在酸性介质中对甲酸的电化学氧化和碱性介质中对异丙醇的电催化氧化。复合材料通过SEM和EDX以及电化学方法进行了表征。相比于电沉积在裸玻碳电极上的钯-金双金属催化剂,所制备的聚对苯/钯-金复合催化剂对异丙醇具有更高的电催化活性和稳定性。另一方面,聚对苯/钯-金复合催化剂对甲酸的电催化活性也得到了很大提高。
5.为了进一步验证聚吲哚对铂催化剂的电催化氧化的促进作用及弄清其促进机理。我们在3.0 mM H2PtCl6 + 0.1 mM吲哚水溶液中通过电化学自组装法一步制备新型的Pt-吲哚复合催化剂。所制备的复合催化剂通过SEM, XPS和电化学方法进行了表征。相比于商业化的JM Pt/C,Pt-吲哚复合催化剂对甲酸的电化学氧化具有更高的催化活性和更强的抗毒化能力。CO的剥离实验结果表明,CO在Pt-吲哚复合催化剂上的吸附强度大大减弱。这可能是因为富电子的吲哚能增加Pt表面的电子结合能和吲哚的吸附使铂表面微结构发生变化所致。
Low-temperature fuel cells as new-style energy devices have attracted great attention because of their high-energy conversion efficiency, low operating temperature, low pollutant emission, the simplicity of handling liquid fuel and quick startup. High efficient electrochemical oxidation of small organic molecules will be directly related to the development and application of low-temperature fuel cells. The current state of the art employs carbon-supported platinum and platinum alloys as anode and cathode catalysts in low-temperature fuel cells. However, carbon material may cause easily Pt particle aggregation and carbon corrosion occurred by electrochemical oxidation, which lower the utilization rate of Pt and the lifetime of fuel cell. Compositing of conducting polymers (CPs) with precious metal possesses some advantages, such as high anti-corrosion, good electron and proton conductivities, and synergistic effect. For the electrooxidation of small organic molecules, presently, CPs as host material of precious metals were centered on the polyaniline, polypyrrole, polythiophene and their derivatives. Electrodepositon had been proved to be one of the most useful approaches for the preparation of conducting polymer and its composites. Other CPs with excellent performances has been developed. Therefore, it would be quite significant to extend such studies to other CPs which might be more suitable as host materials of precious metals in low-temperature fuel cells. In this dissertation, we fabricated a series of novel CPs/metal composites such as Polyindoles/Pt, Polycarbazole/Pt-Ru and Poly(p-phenylene)/Pd-Au, and evaluated the electrooxidation activities of small organic molecules (for example: formic acid, methanol and isopropanol) on the different composite catalysts. Additionally, we systematically studied different parameters affecting the electrooxidation of small organic molecules and the nature of synergistic effect between CP and metal. We also prepared Pt catalyst modified with indole for the high efficient electrooxidation of formic acid. They were briefly described as follows.
1. Four novel composite catalysts have been developed by the electrodeposition of Pt onto glassy carbon electrode (GC) modified with polyindoles: polyindole, poly(5-methoxyindole), poly(5-nitroindole) and poly(5-cyanoindole), which were prepared from boron trifluoride diethyl etherate and its mixed electrolyte. As-formed composite catalysts were characterized by SEM, XRD and electrochemical analysis. Compared with Pt nanoparticles deposited on the GC modified with polypyrrole, the four newly developed composite catalysts exhibited higher catalytic activity towards formic acid electrooxidation by improving selectivity of the reaction via dehydrogenation pathway and thus mostly suppressing the generation of poisonous COads species. The enhanced performance was proposed to come from the synergetic effect between Pt and polyindoles and the increase of electrochemical active surface area (EASA) of Pt on polyindoles. On the other hand, the results of the catalytic activity for methanol oxidation showed that the Pt/PIn/GC and Pt/PMI/GC exhibited higher catalytic activity and stronger poisoning-tolerance than Pt/PPy/GC.
2. Polycarbazole (PCZ) was obtained by the electropolymerization of carbazole in boron trifluoride diethyl etherate + 20% ethyl ether on glassy carbon electrode (GC). The monometallic Pt and bimetallic Pt-Ru nanoparticles firstly dispersed onto PCZ (Pt/PCZ/GC, Pt-Ru/PCZ/GC) and their electro-catalytic activities towards formic acid and methanol oxidation have been investigated. PCZ had good conductibility and electrochemical activity in 0.5 M H2SO4. As-formed electrodes were characterized by SEM, EDS and electrochemical analysis. Relative to Pt and Pt-Ru deposited on the bare GC (Pt/GC, Pt-Ru/GC), Pt/PCZ/GC and Pt-Ru/PCZ/GC had a somewhat enhanced efficiency for the methanol oxidation, however, they exhibited higher catalytic activity and stronger poisoning-tolerance ability towards formic acid electro-oxidation. The enhanced performance was proposed to come from the synergetic effect between metal particles (Pt, Pt-Ru) and PCZ. At the same time, the results of the stripping voltammograms of CO show that PCZ can weaken largely the adsorption strength of CO on catalysts and electro-oxidize COads easily on catalysts.
3. We found that as-prepared poly(5-nitroindole) (PNI) in alkaline solutions had also good electrochemical activity and stability in the potential range from -0.6 to 0.5 V versus SCE. Therefore, we firstly studied the electrooxidation of methanol on Pt/poly(5-nitroindole) (Pt/PNI) in alkaline media. The effects of different parameters related to the methanol oxidation reaction kinetics, such as Pt loading, mass of PNI film, concentration of methanol and KOH, potential scan rate, have been investigated in detail. The results of the catalytic activity for methanol oxidation showed that Pt/PNI had higher catalytic activity and stronger poisoning-tolerance than Pt/GC electrode.
4. Poly(p-phenylene) (PPP) films were synthesized by a low-potential electrochemical polymerization of biphenyl in pure boron trifluoride diethyl etherate. As-formed PPP film was firstly used as a catalyst support. Pd-Au nanoparticles were successfully electro-deposited on PPP films (namely, Pd-Au/PPP) and used for the electrooxidation of isopropanol in alkaline media and the electrooxidation of formic acid in acidic media. As-prepared Pd-Au/PPP composite catalyst was characterized by SEM, EDX and electrochemical methods. The results for isopropanol oxidation indicated that Pd-Au/PPP had higher catalytic activity and stronger poisoning resistance than the Pd-Au deposited on the bare electrode. On the other hand, the electrocatalytic activity of formic acid oxidation on Pd-Au/PPP composite catalyst was also enhanced relative to Pd-Au/GC.
5. In order to further prove the synergistic effect of polyindole and Pt, self-assembly of Pt and indole into a novel composite catalyst on a glassy carbon electrode (GC) has been developed by a one-step electrodeposition in the presence of 3.0 mM H2PtCl6 and 0.1 mM indole. As-formed Pt-indole composite catalyst was characterized by SEM, XPS and the electrochemical methods. Compared to Pt/GC and Pt/C, the novel Pt-indole composite catalyst exhibited higher catalytic activity and stronger poisoning-tolerance for electrooxidation of formic acid. The adsorption strength of CO on Pt-indole composite catalyst was greatly weakened as demonstrated by CO stripping voltammograms. This was due to indole with an abundant amount of electrons may generate an electronic effect when it adsorbs onto Pt surface and the adsorbed indole on Pt surface will modify the Pt surface microstructure. At the same time, the effects of different parameters related to the formic acid oxidation reaction kinetics, such as Pt loading, concentration of formic acid, potential scan rate, have also been investigated in detail.
1.在三氟化硼乙醚及其混合电解质中分别电化学制备聚吲哚、聚(5-甲氧基吲哚)、聚(5-硝基吲哚)、聚(5-氰基吲哚)等导电聚合物,首次以这些聚合物作为铂催化剂载体。制备的聚吲哚衍生物/铂复合材料通过SEM、XRD及其电化学方法进行了表征。相比于传统的聚吡咯/铂复合催化剂,所制备的四种聚吲哚/铂复合催化剂对甲酸具有更高的电催化活性和和抗毒化能力。这种提高的效果主要来自于聚吲哚及其衍生物与铂之间的协同作用和铂的电化学活性位点的增加,这种协调作用促进了甲酸的直接电化学氧化。另一方面,相比于聚吡咯/铂复合催化剂,聚吲哚/Pt和聚(5-甲氧基吲哚)/Pt复合材料对甲醇具有更高的电催化氧化能力和抗毒化能力。
2.在三氟化硼乙醚+ 50%乙醚混合电解质中电化学制备了聚咔唑,首次以聚咔唑为载体负载铂、铂-钌双金属催化剂,详细研究了酸性介质中聚咔唑/铂、聚咔唑/铂-钌复合催化剂对甲酸和甲醇的电化学氧化。聚咔唑在0.5M H2SO4溶液中具有很好的导电性和电化学活性。制备的复合材料通过SEM、EDS和电化学方法进行了表征。相比于电沉积在裸玻碳电极上的铂-钌双金属催化剂,聚咔唑/铂和聚咔唑/铂-钌复合催化剂对甲醇的电化学氧化的促进效果较弱,然而,聚咔唑/铂和聚咔唑/铂-钌复合催化剂对甲酸具有更高的电催化活性和稳定性。这种促进效果可能来自于金属与聚咔唑之间的协同作用。CO的剥离实验结果表明,CO在聚咔唑/铂和聚咔唑/铂-钌复合催化剂上的吸附强度大大减弱、且CO更容易氧化去除。
3.我们发现聚(5-硝基吲哚)在碱性溶液中具有良好的电化学活性和稳定性,因此,我们首次研究了聚(5-硝基吲哚)负载铂催化剂在碱性介质中对甲醇的电化学氧化。详细考察了不同参数对甲醇的电催化氧化的影响,例如:膜的量、铂的载量、KOH和甲醇的浓度、扫描速率和不同的碱性电解质等等。相比于电沉积在裸玻碳电极上的铂催化剂,所制备的聚(5-硝基吲哚)/铂复合催化剂在碱性下对甲醇具有更高的电催化活性和稳定性。
4.在纯三氟化硼乙醚电解质中,以联苯为单体低电位电化学制备了聚对苯,首次以聚对苯为载体成功地负载钯-金双金属催化剂,分别详细研究了聚对苯/钯-金复合催化剂在酸性介质中对甲酸的电化学氧化和碱性介质中对异丙醇的电催化氧化。复合材料通过SEM和EDX以及电化学方法进行了表征。相比于电沉积在裸玻碳电极上的钯-金双金属催化剂,所制备的聚对苯/钯-金复合催化剂对异丙醇具有更高的电催化活性和稳定性。另一方面,聚对苯/钯-金复合催化剂对甲酸的电催化活性也得到了很大提高。
5.为了进一步验证聚吲哚对铂催化剂的电催化氧化的促进作用及弄清其促进机理。我们在3.0 mM H2PtCl6 + 0.1 mM吲哚水溶液中通过电化学自组装法一步制备新型的Pt-吲哚复合催化剂。所制备的复合催化剂通过SEM, XPS和电化学方法进行了表征。相比于商业化的JM Pt/C,Pt-吲哚复合催化剂对甲酸的电化学氧化具有更高的催化活性和更强的抗毒化能力。CO的剥离实验结果表明,CO在Pt-吲哚复合催化剂上的吸附强度大大减弱。这可能是因为富电子的吲哚能增加Pt表面的电子结合能和吲哚的吸附使铂表面微结构发生变化所致。
Low-temperature fuel cells as new-style energy devices have attracted great attention because of their high-energy conversion efficiency, low operating temperature, low pollutant emission, the simplicity of handling liquid fuel and quick startup. High efficient electrochemical oxidation of small organic molecules will be directly related to the development and application of low-temperature fuel cells. The current state of the art employs carbon-supported platinum and platinum alloys as anode and cathode catalysts in low-temperature fuel cells. However, carbon material may cause easily Pt particle aggregation and carbon corrosion occurred by electrochemical oxidation, which lower the utilization rate of Pt and the lifetime of fuel cell. Compositing of conducting polymers (CPs) with precious metal possesses some advantages, such as high anti-corrosion, good electron and proton conductivities, and synergistic effect. For the electrooxidation of small organic molecules, presently, CPs as host material of precious metals were centered on the polyaniline, polypyrrole, polythiophene and their derivatives. Electrodepositon had been proved to be one of the most useful approaches for the preparation of conducting polymer and its composites. Other CPs with excellent performances has been developed. Therefore, it would be quite significant to extend such studies to other CPs which might be more suitable as host materials of precious metals in low-temperature fuel cells. In this dissertation, we fabricated a series of novel CPs/metal composites such as Polyindoles/Pt, Polycarbazole/Pt-Ru and Poly(p-phenylene)/Pd-Au, and evaluated the electrooxidation activities of small organic molecules (for example: formic acid, methanol and isopropanol) on the different composite catalysts. Additionally, we systematically studied different parameters affecting the electrooxidation of small organic molecules and the nature of synergistic effect between CP and metal. We also prepared Pt catalyst modified with indole for the high efficient electrooxidation of formic acid. They were briefly described as follows.
1. Four novel composite catalysts have been developed by the electrodeposition of Pt onto glassy carbon electrode (GC) modified with polyindoles: polyindole, poly(5-methoxyindole), poly(5-nitroindole) and poly(5-cyanoindole), which were prepared from boron trifluoride diethyl etherate and its mixed electrolyte. As-formed composite catalysts were characterized by SEM, XRD and electrochemical analysis. Compared with Pt nanoparticles deposited on the GC modified with polypyrrole, the four newly developed composite catalysts exhibited higher catalytic activity towards formic acid electrooxidation by improving selectivity of the reaction via dehydrogenation pathway and thus mostly suppressing the generation of poisonous COads species. The enhanced performance was proposed to come from the synergetic effect between Pt and polyindoles and the increase of electrochemical active surface area (EASA) of Pt on polyindoles. On the other hand, the results of the catalytic activity for methanol oxidation showed that the Pt/PIn/GC and Pt/PMI/GC exhibited higher catalytic activity and stronger poisoning-tolerance than Pt/PPy/GC.
2. Polycarbazole (PCZ) was obtained by the electropolymerization of carbazole in boron trifluoride diethyl etherate + 20% ethyl ether on glassy carbon electrode (GC). The monometallic Pt and bimetallic Pt-Ru nanoparticles firstly dispersed onto PCZ (Pt/PCZ/GC, Pt-Ru/PCZ/GC) and their electro-catalytic activities towards formic acid and methanol oxidation have been investigated. PCZ had good conductibility and electrochemical activity in 0.5 M H2SO4. As-formed electrodes were characterized by SEM, EDS and electrochemical analysis. Relative to Pt and Pt-Ru deposited on the bare GC (Pt/GC, Pt-Ru/GC), Pt/PCZ/GC and Pt-Ru/PCZ/GC had a somewhat enhanced efficiency for the methanol oxidation, however, they exhibited higher catalytic activity and stronger poisoning-tolerance ability towards formic acid electro-oxidation. The enhanced performance was proposed to come from the synergetic effect between metal particles (Pt, Pt-Ru) and PCZ. At the same time, the results of the stripping voltammograms of CO show that PCZ can weaken largely the adsorption strength of CO on catalysts and electro-oxidize COads easily on catalysts.
3. We found that as-prepared poly(5-nitroindole) (PNI) in alkaline solutions had also good electrochemical activity and stability in the potential range from -0.6 to 0.5 V versus SCE. Therefore, we firstly studied the electrooxidation of methanol on Pt/poly(5-nitroindole) (Pt/PNI) in alkaline media. The effects of different parameters related to the methanol oxidation reaction kinetics, such as Pt loading, mass of PNI film, concentration of methanol and KOH, potential scan rate, have been investigated in detail. The results of the catalytic activity for methanol oxidation showed that Pt/PNI had higher catalytic activity and stronger poisoning-tolerance than Pt/GC electrode.
4. Poly(p-phenylene) (PPP) films were synthesized by a low-potential electrochemical polymerization of biphenyl in pure boron trifluoride diethyl etherate. As-formed PPP film was firstly used as a catalyst support. Pd-Au nanoparticles were successfully electro-deposited on PPP films (namely, Pd-Au/PPP) and used for the electrooxidation of isopropanol in alkaline media and the electrooxidation of formic acid in acidic media. As-prepared Pd-Au/PPP composite catalyst was characterized by SEM, EDX and electrochemical methods. The results for isopropanol oxidation indicated that Pd-Au/PPP had higher catalytic activity and stronger poisoning resistance than the Pd-Au deposited on the bare electrode. On the other hand, the electrocatalytic activity of formic acid oxidation on Pd-Au/PPP composite catalyst was also enhanced relative to Pd-Au/GC.
5. In order to further prove the synergistic effect of polyindole and Pt, self-assembly of Pt and indole into a novel composite catalyst on a glassy carbon electrode (GC) has been developed by a one-step electrodeposition in the presence of 3.0 mM H2PtCl6 and 0.1 mM indole. As-formed Pt-indole composite catalyst was characterized by SEM, XPS and the electrochemical methods. Compared to Pt/GC and Pt/C, the novel Pt-indole composite catalyst exhibited higher catalytic activity and stronger poisoning-tolerance for electrooxidation of formic acid. The adsorption strength of CO on Pt-indole composite catalyst was greatly weakened as demonstrated by CO stripping voltammograms. This was due to indole with an abundant amount of electrons may generate an electronic effect when it adsorbs onto Pt surface and the adsorbed indole on Pt surface will modify the Pt surface microstructure. At the same time, the effects of different parameters related to the formic acid oxidation reaction kinetics, such as Pt loading, concentration of formic acid, potential scan rate, have also been investigated in detail.
引文
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