掺杂纳米碳催化剂的制备及其氧还原催化作用的研究
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摘要
低温燃料电池作为一种洁净能源技术，具有比能量高、工作条件温和、启动速度快等优点，是一种理想的新能源汽车动力电源。目前，低温燃料电池需要在阴极附载大量的铂碳催化剂以加快缓慢的氧还原反应。尽管铂碳催化剂是现有技术水平中氧还原催化活性最好的一类催化剂，然而，铂作为一种贵金属，其不但价格昂贵，而且在自然界中储量稀少。因此，在低温燃料电池阴极中由于使用高载量的铂碳催化剂而导致的高成本及应用的不可持续性一直是低温燃料电池大规模商业化应用的最大障碍。所以，开发出价格低廉且具有较高氧还原催化活性与稳定性的非铂催化剂来替代铂碳催化剂，被认为是降低该类燃料电池成本，最终实现其大规模商业化应用的可行途径。在所有的非铂催化剂中，掺杂碳基催化剂因具有优良的氧还原催化活性、低甲醇渗透影响和高稳定性而吸引了研究者们的广泛兴趣。
本论文以廉价、易得的化合物为原料，通过化学气相沉积法、硬模板加高温分解法、转移掺杂法、软模板加高温分解法等途径制备了具有特殊形貌的掺杂纳米碳基氧还原催化剂。并结合催化剂的形貌、化学组成、微观结构、氧还原催化活性等参数，对催化剂的氧还原催化机理、催化活性的影响因素做了深入地探讨。
首先，以二茂铁和咪唑为前驱物，采用化学气相沉积法制备了掺氮碳纳米管阵列。该掺氮碳纳米管具有约100nm的外径和32层的的管壁，最高氮含量可达8.54at%。作为一种非铂催化剂，此掺氮碳纳米管在0.5M的H_2SO_4溶液与0.1M的KOH溶液中均表现出良好的氧还原催化活性；其中750℃下制备的掺氮碳纳米管氧还原催化活性最高，并且在碱性介质中的活性要优于在酸性介质中的活性。根据催化活性与催化剂表面吡啶型氮含量同步递变的现象，得出了吡啶型氮扮演着氧还原催化活性中心角色的结论。
其次，以Fe2O3纳米粒子为硬模板剂，经过聚苯胺包覆、高温分解、硫酸除杂、高温石墨化处理四道工序，制备了比表面积高达555m2·g-1的泡状掺氮碳材料。尽管该碳材料氮含量低至1.42at%，但其在氧饱和的0.5M H_2SO_4溶液中具有高达0.93V（vs.RHE）的起始电位与0.82V的半波电位，氧还原催化活性可与20wt%的商业Pt/C相媲美。以该泡状掺氮碳材料为阴极催化剂的氢/空质子交换膜单电池在70℃工作温度下具有0.85V的开路电压和191mW·cm2的最大功率密度。我们认为该催化剂的高氧还原催化活性源自于泡状结构产生带来的高催化活性中心密度。此外，我们还认为铁并不是氧还原催化活性中心的有机组成部分，仅起到促进催化活性中心形成的作用。
第三，先以热膨胀法将氧化石墨制成氧化石墨烯，再以聚苯胺为氮源，通过转移掺杂法在850℃下将氧化石墨烯还原、掺杂为掺氮石墨烯。经还原、掺氮后的石墨烯氧含量低至5.17at%，氮含量高达6.25at%,并且具有完整的石墨烯形貌与结构。该掺氮石墨烯在氧饱和的0.1M KOH溶液中起始电位、半波电位、极限电流密度分别为-0.01V、-0.12V (vs. Ag/AgCl)、5.38mA·cm~(-2)，与20wt%的商业Pt/C催化剂具有相等的氧还原电催化活性；并且表现出不受甲醇渗透影响的特性。催化剂的高氧还原催化活性可归功于聚苯胺作为氮原、石墨烯的高比表面及高石墨化、以及石墨烯的一些特殊性能。
,最后，以β-萘磺酸衍生物为软模板剂、苯胺为单体，经过聚合、掺铁、碳化、酸处理、石墨化工序得到具有3D结构的自支撑氮、硫二元掺杂碳纳米纤维网。当反应物中β-萘磺酸的浓度从0.0125M上升到0.05M时，产物由掺杂碳纳米管与碳纳米纤维的共存体系转变为单纯的掺杂碳纤维；并且在材料的长度和直径都有所增加的同时，碳纤维与碳纤维之间还以分枝的方式相互连接形成了三维网状结构。氮含量最高的（4.89wt%）、以苯胺/萘磺酸摩尔比为4:6制备的催化剂，具有最好的氧还原催化活性。当掺入3wt%的铁后，催化剂的氧还原催化活性获得进一步提高，在0.1M的HClO_4中，起始电位达到了0.57V（vs. Ag/AgCl）。此催化剂的高氧还原催化活性被认为归功于氮、硫二元杂原子与碳原子之间的协同效应，以及三维结构导致的氧扩散效率的提高。
Low temperature fuel cells have been recognized as a kind of promising power sourcefor new energy vehicles, due to their advantages such as high power density, low operationtemperature and quick startup. However, high loading of Pt-based catalysts on the cathode isneeded to facilitate the sluggish oxygen reduction reaction (ORR) at the current technologystatus. The high cost and unsustainability of low temperature fuel cells resulting from theexpensive and scarce Pt are becoming one of the most important factors, which block thelarge-scale commercialization of this technology. Thus, developing the inexpensive non-Ptcathodic catalysts with both high performance and durability to substitute Pt-based catalystshas been regarded as a feasible way to reduce the cost of the fuel cells, and to realize theirlarge-scale commercialization. Among all the non-Pt cathodic catalysts, doped carbonmaterials have been widely studied for their high catalytic activity, less sensitivity formethanol cross-over and excellent stability.
In this thesis, doped carbon nanomaterials with unique morphology have been preparedby the chemical vapor deposition method, hard template method, transfer doping method, andsoft template method, with some simple compounds as precursors. The performances andstructural characteristics of the catalysts, the structure of the catalytic active site, and theeffects of some preparation parameters on the catalysts have been investigated extensivelythrough the evaluation and the characterizations. The morphology, composition,microstructure of these catalysts have been revealed.
Firstly, nitrogen-doped carbon nanotubes (N-CNTs) arrays have been prepared by achemical vapor deposition approach, using ferrocene as the catalyst and imidazole as thecarbon and nitrogen precursor. The N-CNTs have about100nm of outside diameter and32wall layers with a bamboo-like structure, the nitrogen content reaches high up to8.54at%.For the reduction of oxygen, the N-CNTs showed excellent electrocatalytic activity in bothacidic medium (0.5M H_2SO_4) and alkaline medium (0.1M KOH), especially in alkalinemedium. The optimum temperature for the preparation of the catalysts, in terms of catalyticactivity, is750C. It is found that the pyridinic nitrogen plays most important role for thecatalyst, it may be the most important components to the catalytic active site.
Secondly, Vesicular nitrogen doped carbon (VNC) material, with BET surface area ofhigh up to555m2·g1, has been prepared by pyrolyzing the polyaniline covering on the Fe_2O_3nanoparticles, followed by acid leaching with H_2SO_4and graphitization. Although thenitrogen content is low, only1.42at%, VNC exhibits excellent catalytic activity towards oxygen reduction reaction comparable to commercial20wt%Pt/C, with the onset potentialand half-wave potential reach to0.93V and0.82V (vs. RHE) in0.5M H2SO4. It isdemonstrated that the air/hydrogen single cell with VNC as cathode catalyst, has anopen-circuit cell potential of0.85V and191mW·cm~(-2)of maximum power density at celltemperature of70C. It is suggested that the high catalytic activity of VNC results from itshigh surface area and high active center density, which may be caused by the vesicularstructure. Furthermore, we believe that the iron may just participate in the construction ofactive sites, but not as a component of the active site.
Thirdly, Well defined nitrogen-doped graphene (NG) has been prepared by a transferdoping approach, in which the graphene oxide (GO) is deoxidized and nitrogen doped by thevaporized polyaniline, and the GO is prepared by a thermal expansion method from graphiteoxide. The content of doped nitrogen in the doped graphene is high up to6.25at%, andoxygen content is lowered to5.17at%. The NG catalyst exhibits excellent activity towardsthe ORR, as well as excellent tolerance towards methanol. In0.1M KOH solution, its onsetpotential, half-wave potential and limiting current density for the ORR are-0.01V,-0.12V(vs. Ag/AgCl) and5.38mA·cm-2, respectively, which are comparable to those of commercial20wt%Pt/C catalyst. It is suggested that the high ORR catalytic activity of NG is attributedto the choice of polianiline as nitrogen source, as well as the large surface area, highgraphitization and special features of NG.
Finally, the3D self-supported N, S-codoped carbon nanofiber network has been preparedby a procedure, including polymerization, addition of Fe, carbonization, acid leaching andgraphitization, with β-naphthalene sulfonic acids (β-NSA), aniline and (NH)_4S_2O_8as startreactants. It was found that the concentration of β-NSA affected the structure of the materialssignificantly. With the concentration of β-NSA increasing from0.0125M to0.05M, thematerials structure is transformed from the coexistence of doped carbon nanotube andnanofiber into pure carbon nanofiber, along with the increase of diameter and length, and theemergence of3D structure. The catalyst derived from the precursor with molai ratio of4:6ofaniline to β-NSA contains highest contents of nitrogen, and shows the best ORR catalyticactivity. Adding3wt%of iron can further enhance the catalytic activity, the onset potential ishigh up to0.57V (vs. Ag/AgCl) in0.1M HClO_4for the material prepared at optimalconditions. It is suggested that the high catalytic activity is attributed to the synergistic effect of nitrogen, sulfur and carbon atoms in the material, as well as the more efficient diffusion ofoxygen in3D codoped carbon nanofiber network.
本论文以廉价、易得的化合物为原料，通过化学气相沉积法、硬模板加高温分解法、转移掺杂法、软模板加高温分解法等途径制备了具有特殊形貌的掺杂纳米碳基氧还原催化剂。并结合催化剂的形貌、化学组成、微观结构、氧还原催化活性等参数，对催化剂的氧还原催化机理、催化活性的影响因素做了深入地探讨。
首先，以二茂铁和咪唑为前驱物，采用化学气相沉积法制备了掺氮碳纳米管阵列。该掺氮碳纳米管具有约100nm的外径和32层的的管壁，最高氮含量可达8.54at%。作为一种非铂催化剂，此掺氮碳纳米管在0.5M的H_2SO_4溶液与0.1M的KOH溶液中均表现出良好的氧还原催化活性；其中750℃下制备的掺氮碳纳米管氧还原催化活性最高，并且在碱性介质中的活性要优于在酸性介质中的活性。根据催化活性与催化剂表面吡啶型氮含量同步递变的现象，得出了吡啶型氮扮演着氧还原催化活性中心角色的结论。
其次，以Fe2O3纳米粒子为硬模板剂，经过聚苯胺包覆、高温分解、硫酸除杂、高温石墨化处理四道工序，制备了比表面积高达555m2·g-1的泡状掺氮碳材料。尽管该碳材料氮含量低至1.42at%，但其在氧饱和的0.5M H_2SO_4溶液中具有高达0.93V（vs.RHE）的起始电位与0.82V的半波电位，氧还原催化活性可与20wt%的商业Pt/C相媲美。以该泡状掺氮碳材料为阴极催化剂的氢/空质子交换膜单电池在70℃工作温度下具有0.85V的开路电压和191mW·cm2的最大功率密度。我们认为该催化剂的高氧还原催化活性源自于泡状结构产生带来的高催化活性中心密度。此外，我们还认为铁并不是氧还原催化活性中心的有机组成部分，仅起到促进催化活性中心形成的作用。
第三，先以热膨胀法将氧化石墨制成氧化石墨烯，再以聚苯胺为氮源，通过转移掺杂法在850℃下将氧化石墨烯还原、掺杂为掺氮石墨烯。经还原、掺氮后的石墨烯氧含量低至5.17at%，氮含量高达6.25at%,并且具有完整的石墨烯形貌与结构。该掺氮石墨烯在氧饱和的0.1M KOH溶液中起始电位、半波电位、极限电流密度分别为-0.01V、-0.12V (vs. Ag/AgCl)、5.38mA·cm~(-2)，与20wt%的商业Pt/C催化剂具有相等的氧还原电催化活性；并且表现出不受甲醇渗透影响的特性。催化剂的高氧还原催化活性可归功于聚苯胺作为氮原、石墨烯的高比表面及高石墨化、以及石墨烯的一些特殊性能。
,最后，以β-萘磺酸衍生物为软模板剂、苯胺为单体，经过聚合、掺铁、碳化、酸处理、石墨化工序得到具有3D结构的自支撑氮、硫二元掺杂碳纳米纤维网。当反应物中β-萘磺酸的浓度从0.0125M上升到0.05M时，产物由掺杂碳纳米管与碳纳米纤维的共存体系转变为单纯的掺杂碳纤维；并且在材料的长度和直径都有所增加的同时，碳纤维与碳纤维之间还以分枝的方式相互连接形成了三维网状结构。氮含量最高的（4.89wt%）、以苯胺/萘磺酸摩尔比为4:6制备的催化剂，具有最好的氧还原催化活性。当掺入3wt%的铁后，催化剂的氧还原催化活性获得进一步提高，在0.1M的HClO_4中，起始电位达到了0.57V（vs. Ag/AgCl）。此催化剂的高氧还原催化活性被认为归功于氮、硫二元杂原子与碳原子之间的协同效应，以及三维结构导致的氧扩散效率的提高。
Low temperature fuel cells have been recognized as a kind of promising power sourcefor new energy vehicles, due to their advantages such as high power density, low operationtemperature and quick startup. However, high loading of Pt-based catalysts on the cathode isneeded to facilitate the sluggish oxygen reduction reaction (ORR) at the current technologystatus. The high cost and unsustainability of low temperature fuel cells resulting from theexpensive and scarce Pt are becoming one of the most important factors, which block thelarge-scale commercialization of this technology. Thus, developing the inexpensive non-Ptcathodic catalysts with both high performance and durability to substitute Pt-based catalystshas been regarded as a feasible way to reduce the cost of the fuel cells, and to realize theirlarge-scale commercialization. Among all the non-Pt cathodic catalysts, doped carbonmaterials have been widely studied for their high catalytic activity, less sensitivity formethanol cross-over and excellent stability.
In this thesis, doped carbon nanomaterials with unique morphology have been preparedby the chemical vapor deposition method, hard template method, transfer doping method, andsoft template method, with some simple compounds as precursors. The performances andstructural characteristics of the catalysts, the structure of the catalytic active site, and theeffects of some preparation parameters on the catalysts have been investigated extensivelythrough the evaluation and the characterizations. The morphology, composition,microstructure of these catalysts have been revealed.
Firstly, nitrogen-doped carbon nanotubes (N-CNTs) arrays have been prepared by achemical vapor deposition approach, using ferrocene as the catalyst and imidazole as thecarbon and nitrogen precursor. The N-CNTs have about100nm of outside diameter and32wall layers with a bamboo-like structure, the nitrogen content reaches high up to8.54at%.For the reduction of oxygen, the N-CNTs showed excellent electrocatalytic activity in bothacidic medium (0.5M H_2SO_4) and alkaline medium (0.1M KOH), especially in alkalinemedium. The optimum temperature for the preparation of the catalysts, in terms of catalyticactivity, is750C. It is found that the pyridinic nitrogen plays most important role for thecatalyst, it may be the most important components to the catalytic active site.
Secondly, Vesicular nitrogen doped carbon (VNC) material, with BET surface area ofhigh up to555m2·g1, has been prepared by pyrolyzing the polyaniline covering on the Fe_2O_3nanoparticles, followed by acid leaching with H_2SO_4and graphitization. Although thenitrogen content is low, only1.42at%, VNC exhibits excellent catalytic activity towards oxygen reduction reaction comparable to commercial20wt%Pt/C, with the onset potentialand half-wave potential reach to0.93V and0.82V (vs. RHE) in0.5M H2SO4. It isdemonstrated that the air/hydrogen single cell with VNC as cathode catalyst, has anopen-circuit cell potential of0.85V and191mW·cm~(-2)of maximum power density at celltemperature of70C. It is suggested that the high catalytic activity of VNC results from itshigh surface area and high active center density, which may be caused by the vesicularstructure. Furthermore, we believe that the iron may just participate in the construction ofactive sites, but not as a component of the active site.
Thirdly, Well defined nitrogen-doped graphene (NG) has been prepared by a transferdoping approach, in which the graphene oxide (GO) is deoxidized and nitrogen doped by thevaporized polyaniline, and the GO is prepared by a thermal expansion method from graphiteoxide. The content of doped nitrogen in the doped graphene is high up to6.25at%, andoxygen content is lowered to5.17at%. The NG catalyst exhibits excellent activity towardsthe ORR, as well as excellent tolerance towards methanol. In0.1M KOH solution, its onsetpotential, half-wave potential and limiting current density for the ORR are-0.01V,-0.12V(vs. Ag/AgCl) and5.38mA·cm-2, respectively, which are comparable to those of commercial20wt%Pt/C catalyst. It is suggested that the high ORR catalytic activity of NG is attributedto the choice of polianiline as nitrogen source, as well as the large surface area, highgraphitization and special features of NG.
Finally, the3D self-supported N, S-codoped carbon nanofiber network has been preparedby a procedure, including polymerization, addition of Fe, carbonization, acid leaching andgraphitization, with β-naphthalene sulfonic acids (β-NSA), aniline and (NH)_4S_2O_8as startreactants. It was found that the concentration of β-NSA affected the structure of the materialssignificantly. With the concentration of β-NSA increasing from0.0125M to0.05M, thematerials structure is transformed from the coexistence of doped carbon nanotube andnanofiber into pure carbon nanofiber, along with the increase of diameter and length, and theemergence of3D structure. The catalyst derived from the precursor with molai ratio of4:6ofaniline to β-NSA contains highest contents of nitrogen, and shows the best ORR catalyticactivity. Adding3wt%of iron can further enhance the catalytic activity, the onset potential ishigh up to0.57V (vs. Ag/AgCl) in0.1M HClO_4for the material prepared at optimalconditions. It is suggested that the high catalytic activity is attributed to the synergistic effect of nitrogen, sulfur and carbon atoms in the material, as well as the more efficient diffusion ofoxygen in3D codoped carbon nanofiber network.
引文
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