多元多尺度氧气还原电催化材料的结构调控与功能化
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摘要
氧气还原反应是一种重要的基本电化学反应，在燃料电池，金属-空气电池，氯碱工业及腐蚀防护等实际工业生产方面具有极为重要的应用。但由于氧气还原反应速率缓慢，过电位高，过程机理复杂，很难在平衡电势附近获得较高的催化电流。因此在实际应用中，必须采用适当的催化剂材料来降低其过电位，提高其反应速率及效率，才能体现出其相应的价值。目前，应用于氧气还原反应的电催化材料主要是炭黑负载贵金属纳米粒子复合催化剂，由于成本较高，稳定性较低，大大限制了其作为商业催化剂的开发应用。因此，设计制备具有高活性、高稳定性的氧气还原反应催化材料对于推进相关领域的研究具有重大的意义。
本论文以负载型催化剂为研究对象，将纳米级金属、金属合金、金属-碳化物及金属硫化物等具有特定催化效果的粒子以特定的纳米结构复合负载在多尺寸纳米炭材料表面来制备多元多尺度电催化材料，利用催化体系的协同效应选择性地控制氧气还原反应的路径，从而提高其反应效率。通过对多尺度多元催化材料对于氧气还原反应电催化性能及机理的研究，揭示炭载体多尺度效应与纳米氧还原电催化材料性质之间的对应关系，多元催化剂之间的协同效应以及多元催化剂与炭载体之间的复合效应，实现多元多尺度氧气还原电化学催化材料的结构调控，并得到了设计高活性氧气还原催化剂的普适原则。取得的主要研究成果如下：
(1)以铂金属纳米粒子作为催化活性中心，选取炭微球，碳纳米管，炭纤维，生物基分级多孔炭等几种具有代表性的炭材料作为载体，通过物理或化学的方法对其进行修饰并与铂粒子复合形成负载型催化剂。根据对其催化氧气还原反应的性能进行比较，揭示了炭载体的结构特征对于催化剂材料催化活性及机理的影响：石墨化程度的提高使载体材料的炭层结构规整度提高，负载金属纳米粒子后形成的复合催化剂参加电化学反应时的起始电位虽然提升不大，但具有较大的催化电流密度，从一定程度上提高了催化剂的催化活性。载体材料的表面状态直接影响到活性中心粒子的负载情况，从而对复合催化剂的催化活性及机理产生影响。以生物材料作为前驱体制备的分级多孔炭材料表面含有大量的官能团，不仅能够使活性中心粒子均匀分散，其表面掺杂的少量氮原子还可以直接参与氧气还原反应。其独特的三维立体分级多孔结构能够促进反应过程中的物质传递过程，从而提高其催化活性。较高的石墨化程度；较大的比表面积；表面具有一定的活性，具有多种可供反应的含氧、氮等元素的活性基团，或者实现氮原子在石墨层结构中的掺杂；以及具有大孔-微孔-介孔的三维立体分级多孔结构，是设计高活性催化剂载体材料的普适原则。
(2)在上述研究的基础上，选取了石墨化程度类似，但尺度不同且具有代表性的四种炭材料作为铂粒子的载体，深入探究复合催化剂对氧气还原反应的催化机理，包括其反应电子数，交换电流密度等参数的比较，揭示了载体的尺度效应对其催化性能及机理的影响：宏观及微观的一维结构有利于电子的集中传递，减少了其他方向上分流，如碳纳米管，炭纤维编织的平面毛毡等，其作为载体材料制备所得的复合催化剂在酸性及碱性溶液中均表现出较高的催化活性及选择性。具有三维立体结构的生物基分级多孔炭载体材料的整流作用虽然不及一维的线状结构，但其对于氧气还原反应的促进作用主要体现在分层及分级孔径分布对反应传质过程的改善和促进。
(3)选取碳纳米管作为载体材料，以铂，金核壳，合金及分相等不同的结构作为活性中心粒子，制备复合催化剂并对其氧气还原反应催化性能进行了研究。结果证明，其催化活性排序如下：核壳结构>合金结构>分相结构。通过对不同铂，金复合结构催化剂催化过程机理的研究可知，核壳结构主要依靠两种金属的协同效应来提高其电催化性能，合金结构是由于表面原子层排列的改变而引起了氧气亲和力的改变，通过影响氧气的吸附过程来提高催化剂的活性，而对于两者分相结构来说，两种金属之间的作用力较弱，因此电催化性能较差，主要依靠能够在金粒子表面负载的铂纳米粒子来完成对氧气还原反应的催化过程。以铂，铁合金作为研究对象，对所得合金粒子进行不同温度的热处理，进一步得出了合金晶体结构对于其催化性能的影响。随着热处理温度的提高，铁铂合金由面心立方的固溶体结构逐渐向FePt3及FePt金属间化合物的结构转变。FePt金属间化合物对于氧气还原反应催化性能的促进作用较强，但当FePt3与固溶体形成混合结构时，能够得到最高的催化活性。
(4)为进一步降低催化材料的成本，提高其稳定性，选择静电纺丝法制备的碳化钛及碳化钨纤维与铂粒子进行复合来制备催化剂。碳化钛及碳化钨均以粒子状态分布于杂乱炭层结构组成的纤维中，编织形成了类似于炭纤维毛毡的平面结构。碳化钛的颗粒约为50nm，部分埋伏在炭层结构中，而碳化钨粒子的粒径则小于5nm，基本全部埋伏于炭层中。铂纳米粒子可以通过化学法而均匀负载于纤维的表面，其催化活性通过与碳化物表面的电子转移作用而得到了一定程度的提高。由于铂粒子与碳化钛颗粒直接接触，电子传递损失较小，而铂粒子与碳化钨则是通过炭层结构间接相连，因此碳化钛对于铂粒子催化氧气还原过程的促进作用优于碳化钨纤维。此外，碳化钨及碳化钛本身在碱性溶液中具有催化氧气还原反应通过四电子途径进行的特性，具有替代贵金属作为催化剂的潜力。
(5)通过对碳纳米管进行表面敏化活化处理，成功的将钴-硫化合物负载于其表面，制备了一种非贵金属氧气还原反应催化剂。经过适当的热处理，得到了多种晶体结构混合而成的钴-硫化合物活性中心粒子，主要为Co9S8及Co3S4的混合。通过对热处理前后及不同钴-硫比例的催化剂催化氧气还原反应性能及机理进行研究，证明了该催化剂主要催化氧气还原反应通过四电子反应途径进行，且Co9S8的晶体组分能够有效的促进复合催化剂的催化性能。
The oxygen reduction reaction (ORR) is an important electrochemicalreaction, which is widely applied in the fuel cells, metal-air batteries,chlor-alkali industry and corrosions. However, the sluggish kinetics of theORR resulted from the high overpotential, complicated process and smallexchange current density, limits the practical applications. As a result, weshould introduce some electrocatalysts to lower the overpotential and improvethe reaction efficiency of the ORR process. Carbon supported platinum (Pt/C)is now developed as the catalysts for the ORR process, but the high cost andlack of stability highly limit the applications as the commercial catalysts forthe devices. Thus, the design of new electrocatalysts with high catalyticactivity and stability is quite a demanding task for the investigations of theORR process.
This thesis mainly focused on the supported electrocatalysts for the ORRprocess, applying metal, metal alloy, metal-carbide, and non-metalmetal-sulfide nanoparticles supported on various carbon materials in order toobtain the multi-phase multi-scale electrocatalysts, which could promote thereaction rates and efficiency of the ORR process. The influences of the support material sizes, various compositions of the catalytic nanoparticles, andthe synergetic effects between the support materials were investigated byanalyzing the activity and mechanism of the multi-scale multi-phaseelectrocatalysts for the ORR process. The controlled synthesis ofelectrocatalysts was accomplished, and some principles for the design of highefficiency electrocatalysts towards the ORR process were also investigated.The main achievements are listed as below:
(1) Platinum (Pt) nanoparticles supported on carbon materials with variousmorphologies and structures, such as carbon spheres, carbon nanotubes,carbon fiber mats and hierarchical porous carbons fabricated frombio-materials were synthesized and applied as the electrocatalysts for the ORRprocess. High graphitization of the carbon materials could improve theregularity of the graphite sheets, and catalytic activities for the ORR process interms of current densities. The surface state of support materials alsoinfluenced the catalytic properties of the electrocatalysts. The hierarchicalporous carbons (HPC) fabricated from the bio-materials possessed not onlyhigh surface areas, but also large amounts of surface functional groups, whichcould make the nanoparticles highly dispersed. Some nitrogen atoms insertedinto the frameworks of the carbons and improved the catalytic activities of theHPC supported electrocatalysts. The principles of the support materials for thehighly active electrocatalysts were high graphitization and surface area;certain amounts of surface functional groups or nitrogen atoms doped on the surface carbon frameworks; hierarchical porous structures which couldpromote the mass transportation.
(2) Several carbon materials with similar graphitization but different sizesand morphologies were selected as the support materials for the Ptnanoparticles. The multi-scale effect of the support materials to the ORRprocess was further analyzed by investigating the mechanism of the reaction,including calculating the numbers transferred during the process and theexchange current densities. The results indicated that the one-dimensionalcarbon materials in macroscopic and microscopic scales, such as carbonnanotubes and carbon fibrous mats, could help the charge transformationduring the catalytic process, which made the corresponding electrocatalystsexhibit high catalytic activity, as well as good selectivity for the ORR process.The promotion effects of three-dimensional HPC support material mainly liedin the influence of the hierarchical porous structures to the mass transportationduring the ORR process.
(3) The carbon nanotube supported Pt-gold (Au) nanoparticles, includingcore-shell, alloy and segregated, were synthesized and their catalyticproperties were characterized. The result indicated that the Pt-Au core-shellstructure exhibited better catalytic activity than the alloy and segregatedstructures. Through the analysis of the ORR mechanisms, we found that thecore-shell structures could improve the catalytic activity through thesynergetic effects between the two metals. In the case of Pt-Au alloy, the surface structures of the nanoparticles changed, and the affinity of the oxygenwas also strengthened. The synergetic effects between Pt and Au was quiteweak in the Pt-Au segregated structures, thus the ORR catalytic process wasmainly accomplished by the Pt nanoparticles supported on the Au particles. Inorder to further analyze the crystalline structure effects to the electrocatalyticactivity for the ORR process, Pt-Ion (Fe) alloy nanoparticles supported oncarbon nanotubes were synthesized and heat-treated at different temperatures.As the temperature increased, the crystalline structures of Pt-Fe alloytransformed from face centered cubic solid solution to the intermetalliccompounds of FePt3or FePt. The result indicated that FePt compound washighly active for the ORR process, but the highest activity was obtained withthe mixture of solid solution and FePt3structure.
(4) In order to further reduce the cost and improve the stability of theelectrocatalysts, the TiC and WC fibrous mats were compound with Ptnanoparticles and applied as the electrocatalysts for the ORR process. The TiCand WC particles were insert into the carbon sheets to form the fibers andinterwoven to form the fibrous mat. TiC particles partially inserted in thecarbon sheets with the diameter of~50nm while the WC particles fullyinserted with the diameter of~5nm. Pt nanoparticles could be highlydispersed on the surface of the fibers, and the catalytic activities wereimproved through the surface charge transformation. The enhancement of TiCfibers was more significant than the WC fibers due to the direct contact between the Pt and TiC particles instead of interconnect though the carbonatoms. Furthermore, the TiC and WC fibers also exhibited certain catalyticactivities in the alkaline solutions through the four-electron pathway, whichmight be developed as an alternative electrocatalysts of the metal materials.
(5) The non-metal cobalt-sulfur compounds supported on the carbonnanotubes were synthesized after sensitizing and activating the surface of thesupport materials. Through the appropriate heat-treatment, the cobalt-sulfurparticles changed to the mixture of mainly Co9S8and Co3S4, and the catalyticactivities and mechanism before and after the heat-treatment were compared.The results indicated that the carbon nanotube supported cobalt-sulfur particlemainly catalyzed the ORR proceed through the four-electron pathway and theCo9S8could highly improve the catalytic activities compared with the othercompounds.
本论文以负载型催化剂为研究对象，将纳米级金属、金属合金、金属-碳化物及金属硫化物等具有特定催化效果的粒子以特定的纳米结构复合负载在多尺寸纳米炭材料表面来制备多元多尺度电催化材料，利用催化体系的协同效应选择性地控制氧气还原反应的路径，从而提高其反应效率。通过对多尺度多元催化材料对于氧气还原反应电催化性能及机理的研究，揭示炭载体多尺度效应与纳米氧还原电催化材料性质之间的对应关系，多元催化剂之间的协同效应以及多元催化剂与炭载体之间的复合效应，实现多元多尺度氧气还原电化学催化材料的结构调控，并得到了设计高活性氧气还原催化剂的普适原则。取得的主要研究成果如下：
(1)以铂金属纳米粒子作为催化活性中心，选取炭微球，碳纳米管，炭纤维，生物基分级多孔炭等几种具有代表性的炭材料作为载体，通过物理或化学的方法对其进行修饰并与铂粒子复合形成负载型催化剂。根据对其催化氧气还原反应的性能进行比较，揭示了炭载体的结构特征对于催化剂材料催化活性及机理的影响：石墨化程度的提高使载体材料的炭层结构规整度提高，负载金属纳米粒子后形成的复合催化剂参加电化学反应时的起始电位虽然提升不大，但具有较大的催化电流密度，从一定程度上提高了催化剂的催化活性。载体材料的表面状态直接影响到活性中心粒子的负载情况，从而对复合催化剂的催化活性及机理产生影响。以生物材料作为前驱体制备的分级多孔炭材料表面含有大量的官能团，不仅能够使活性中心粒子均匀分散，其表面掺杂的少量氮原子还可以直接参与氧气还原反应。其独特的三维立体分级多孔结构能够促进反应过程中的物质传递过程，从而提高其催化活性。较高的石墨化程度；较大的比表面积；表面具有一定的活性，具有多种可供反应的含氧、氮等元素的活性基团，或者实现氮原子在石墨层结构中的掺杂；以及具有大孔-微孔-介孔的三维立体分级多孔结构，是设计高活性催化剂载体材料的普适原则。
(2)在上述研究的基础上，选取了石墨化程度类似，但尺度不同且具有代表性的四种炭材料作为铂粒子的载体，深入探究复合催化剂对氧气还原反应的催化机理，包括其反应电子数，交换电流密度等参数的比较，揭示了载体的尺度效应对其催化性能及机理的影响：宏观及微观的一维结构有利于电子的集中传递，减少了其他方向上分流，如碳纳米管，炭纤维编织的平面毛毡等，其作为载体材料制备所得的复合催化剂在酸性及碱性溶液中均表现出较高的催化活性及选择性。具有三维立体结构的生物基分级多孔炭载体材料的整流作用虽然不及一维的线状结构，但其对于氧气还原反应的促进作用主要体现在分层及分级孔径分布对反应传质过程的改善和促进。
(3)选取碳纳米管作为载体材料，以铂，金核壳，合金及分相等不同的结构作为活性中心粒子，制备复合催化剂并对其氧气还原反应催化性能进行了研究。结果证明，其催化活性排序如下：核壳结构>合金结构>分相结构。通过对不同铂，金复合结构催化剂催化过程机理的研究可知，核壳结构主要依靠两种金属的协同效应来提高其电催化性能，合金结构是由于表面原子层排列的改变而引起了氧气亲和力的改变，通过影响氧气的吸附过程来提高催化剂的活性，而对于两者分相结构来说，两种金属之间的作用力较弱，因此电催化性能较差，主要依靠能够在金粒子表面负载的铂纳米粒子来完成对氧气还原反应的催化过程。以铂，铁合金作为研究对象，对所得合金粒子进行不同温度的热处理，进一步得出了合金晶体结构对于其催化性能的影响。随着热处理温度的提高，铁铂合金由面心立方的固溶体结构逐渐向FePt3及FePt金属间化合物的结构转变。FePt金属间化合物对于氧气还原反应催化性能的促进作用较强，但当FePt3与固溶体形成混合结构时，能够得到最高的催化活性。
(4)为进一步降低催化材料的成本，提高其稳定性，选择静电纺丝法制备的碳化钛及碳化钨纤维与铂粒子进行复合来制备催化剂。碳化钛及碳化钨均以粒子状态分布于杂乱炭层结构组成的纤维中，编织形成了类似于炭纤维毛毡的平面结构。碳化钛的颗粒约为50nm，部分埋伏在炭层结构中，而碳化钨粒子的粒径则小于5nm，基本全部埋伏于炭层中。铂纳米粒子可以通过化学法而均匀负载于纤维的表面，其催化活性通过与碳化物表面的电子转移作用而得到了一定程度的提高。由于铂粒子与碳化钛颗粒直接接触，电子传递损失较小，而铂粒子与碳化钨则是通过炭层结构间接相连，因此碳化钛对于铂粒子催化氧气还原过程的促进作用优于碳化钨纤维。此外，碳化钨及碳化钛本身在碱性溶液中具有催化氧气还原反应通过四电子途径进行的特性，具有替代贵金属作为催化剂的潜力。
(5)通过对碳纳米管进行表面敏化活化处理，成功的将钴-硫化合物负载于其表面，制备了一种非贵金属氧气还原反应催化剂。经过适当的热处理，得到了多种晶体结构混合而成的钴-硫化合物活性中心粒子，主要为Co9S8及Co3S4的混合。通过对热处理前后及不同钴-硫比例的催化剂催化氧气还原反应性能及机理进行研究，证明了该催化剂主要催化氧气还原反应通过四电子反应途径进行，且Co9S8的晶体组分能够有效的促进复合催化剂的催化性能。
The oxygen reduction reaction (ORR) is an important electrochemicalreaction, which is widely applied in the fuel cells, metal-air batteries,chlor-alkali industry and corrosions. However, the sluggish kinetics of theORR resulted from the high overpotential, complicated process and smallexchange current density, limits the practical applications. As a result, weshould introduce some electrocatalysts to lower the overpotential and improvethe reaction efficiency of the ORR process. Carbon supported platinum (Pt/C)is now developed as the catalysts for the ORR process, but the high cost andlack of stability highly limit the applications as the commercial catalysts forthe devices. Thus, the design of new electrocatalysts with high catalyticactivity and stability is quite a demanding task for the investigations of theORR process.
This thesis mainly focused on the supported electrocatalysts for the ORRprocess, applying metal, metal alloy, metal-carbide, and non-metalmetal-sulfide nanoparticles supported on various carbon materials in order toobtain the multi-phase multi-scale electrocatalysts, which could promote thereaction rates and efficiency of the ORR process. The influences of the support material sizes, various compositions of the catalytic nanoparticles, andthe synergetic effects between the support materials were investigated byanalyzing the activity and mechanism of the multi-scale multi-phaseelectrocatalysts for the ORR process. The controlled synthesis ofelectrocatalysts was accomplished, and some principles for the design of highefficiency electrocatalysts towards the ORR process were also investigated.The main achievements are listed as below:
(1) Platinum (Pt) nanoparticles supported on carbon materials with variousmorphologies and structures, such as carbon spheres, carbon nanotubes,carbon fiber mats and hierarchical porous carbons fabricated frombio-materials were synthesized and applied as the electrocatalysts for the ORRprocess. High graphitization of the carbon materials could improve theregularity of the graphite sheets, and catalytic activities for the ORR process interms of current densities. The surface state of support materials alsoinfluenced the catalytic properties of the electrocatalysts. The hierarchicalporous carbons (HPC) fabricated from the bio-materials possessed not onlyhigh surface areas, but also large amounts of surface functional groups, whichcould make the nanoparticles highly dispersed. Some nitrogen atoms insertedinto the frameworks of the carbons and improved the catalytic activities of theHPC supported electrocatalysts. The principles of the support materials for thehighly active electrocatalysts were high graphitization and surface area;certain amounts of surface functional groups or nitrogen atoms doped on the surface carbon frameworks; hierarchical porous structures which couldpromote the mass transportation.
(2) Several carbon materials with similar graphitization but different sizesand morphologies were selected as the support materials for the Ptnanoparticles. The multi-scale effect of the support materials to the ORRprocess was further analyzed by investigating the mechanism of the reaction,including calculating the numbers transferred during the process and theexchange current densities. The results indicated that the one-dimensionalcarbon materials in macroscopic and microscopic scales, such as carbonnanotubes and carbon fibrous mats, could help the charge transformationduring the catalytic process, which made the corresponding electrocatalystsexhibit high catalytic activity, as well as good selectivity for the ORR process.The promotion effects of three-dimensional HPC support material mainly liedin the influence of the hierarchical porous structures to the mass transportationduring the ORR process.
(3) The carbon nanotube supported Pt-gold (Au) nanoparticles, includingcore-shell, alloy and segregated, were synthesized and their catalyticproperties were characterized. The result indicated that the Pt-Au core-shellstructure exhibited better catalytic activity than the alloy and segregatedstructures. Through the analysis of the ORR mechanisms, we found that thecore-shell structures could improve the catalytic activity through thesynergetic effects between the two metals. In the case of Pt-Au alloy, the surface structures of the nanoparticles changed, and the affinity of the oxygenwas also strengthened. The synergetic effects between Pt and Au was quiteweak in the Pt-Au segregated structures, thus the ORR catalytic process wasmainly accomplished by the Pt nanoparticles supported on the Au particles. Inorder to further analyze the crystalline structure effects to the electrocatalyticactivity for the ORR process, Pt-Ion (Fe) alloy nanoparticles supported oncarbon nanotubes were synthesized and heat-treated at different temperatures.As the temperature increased, the crystalline structures of Pt-Fe alloytransformed from face centered cubic solid solution to the intermetalliccompounds of FePt3or FePt. The result indicated that FePt compound washighly active for the ORR process, but the highest activity was obtained withthe mixture of solid solution and FePt3structure.
(4) In order to further reduce the cost and improve the stability of theelectrocatalysts, the TiC and WC fibrous mats were compound with Ptnanoparticles and applied as the electrocatalysts for the ORR process. The TiCand WC particles were insert into the carbon sheets to form the fibers andinterwoven to form the fibrous mat. TiC particles partially inserted in thecarbon sheets with the diameter of~50nm while the WC particles fullyinserted with the diameter of~5nm. Pt nanoparticles could be highlydispersed on the surface of the fibers, and the catalytic activities wereimproved through the surface charge transformation. The enhancement of TiCfibers was more significant than the WC fibers due to the direct contact between the Pt and TiC particles instead of interconnect though the carbonatoms. Furthermore, the TiC and WC fibers also exhibited certain catalyticactivities in the alkaline solutions through the four-electron pathway, whichmight be developed as an alternative electrocatalysts of the metal materials.
(5) The non-metal cobalt-sulfur compounds supported on the carbonnanotubes were synthesized after sensitizing and activating the surface of thesupport materials. Through the appropriate heat-treatment, the cobalt-sulfurparticles changed to the mixture of mainly Co9S8and Co3S4, and the catalyticactivities and mechanism before and after the heat-treatment were compared.The results indicated that the carbon nanotube supported cobalt-sulfur particlemainly catalyzed the ORR proceed through the four-electron pathway and theCo9S8could highly improve the catalytic activities compared with the othercompounds.
引文
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