氧还原方法学及其催化剂研究
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摘要
质子交换膜燃料电池技术能在室温附近直接将化学能高效地转换为电能,运行时几乎不排放或仅排放少量污染物。自1960年代以来,该技术一直被世界各国重视。但是该技术目前尚未实现大规模的商品化。在性能最好的铂基催化剂上,氧电催化还原的起始超电势依然在0.25V以上。氧的阴极还原反应动力学很慢,超电势高是限制燃料电池输出功率与能量效率的瓶颈。理解氧还原反应的机理、了解影响其反应动力学的关键因素以及提高催化剂的氧还原活性,是燃料电池电催化领域的重要研究课题。虽然经过半个多世纪对研究,人们对氧电极反应取得了很多原子、分子水平上的认识,但是对氧还原的高超电势的起源、催化剂的氧还原活性与结构的内在关系等问题,依然还没有清晰的认识。其主要原因是一方面氧还原反应是一个涉及4电子转移、多步骤的复杂反应,人们在研究中并没有仔细考究常用于研究纳米电催化剂的氧还原反应活性的薄膜旋转圆盘电极技术是否切实可靠。针对上述问题,本论文开展了以下工作：
1.表征氧还原电催化剂活性的实验方法验证。由于溶液中,氧气的溶解度低,电极反应必然会受到溶液相以及催化剂层内传质的影响。同时,未补偿溶液电阻也会对估算的超电势带来影响。如何完全排除传质以及溶液内阻的影响,并获得电催化剂对氧还原反应的内在活性,是讨论氧还原催化剂的构、效关系的前提。本论文首先系统考察了溶液内阻对氧还原动力学测量的影响,并讨论了文献中有关论文在该问题上可能存在的误导,在此基础上提出了正确的溶液内阻补偿方法；然后系统地考察了催化剂的担载量,反应物在催化剂层中的传质对利用薄膜旋转圆盘电极技术获取氧还原动力学数据的影响,指出了正确利用该技术合理评价氧还原电极反应的内在活性的注意事项。
2.为了弄清铂基催化剂上氧还原的高超电势的起源,我们系统研究电解质溶液的pH值对Pt电极上H和OH的吸、脱附反应：尤其是OHad+H++e(?)H20(酸性介质)或者OHad+e(?)OH-(碱性介质)以及氧还原动力学的影响。我们发现i)在氧还原的动力学以及动力学与传质混合控制的电位区,上述反应即是氧电催化还原反应的最后一步,又是与氧还原平行进行、竞争反应活性位点的另一个可逆反应。而且,OHad的脱附动力学非常快,OHad的覆盖度主要受热力学因素决定；ⅱ)影响氧还原动力学的关键因素是在氧还原电位区与OH吸、脱附的热力学以及动力学。一方面,OH吸、脱附可逆发生的上限电位,决定了氧还原的起始电位,OHad的覆盖度限制了用于氧还原的活性位点数：另一方面,OHad脱附作为电催化氧还原反应的最后一步,而OHad+H++e(?)H2O或OHad+e(?)OH-在氧还原的动力学与传质混合控制的电位区可逆地向着两个方向同时进行,也限制了氧还原的净速度。在此基础上,我们还尝试制备了二元的PtxY催化剂,也证实了上述观点。
Proton exchange membrane fuel cells which can directly converted chemical energy into electrical energy near room temperature, and emit almost no or just a small amount of pollutants. Therefore, since the1960s, the R&D of such fuel cells has been greatly supported worldwide. However, by now such fuel cells have been successfully commercialized on large scale. Wherein an important bottleneck is that the kinetics for oxygen cathode reaction is very slow. Understanding the mechanism of the oxygen reduction reaction (ORR) has been one of the important research topic in the fuel cell catalysis, at the best Pt based electrocatalysts available so far, the overpotential at the onset for ORR is still as high as0.25V. After60years of research, much atomic, molecular level understanding for ORR has been gained. However, no consensus on ORR mechanism and key factors which limits ORR kinetics has been reached so far.This is probably due to, on one hand, ORR is a reaction involves4electron, multiple step complex process, on the other hand, some misunderstanding exists on using thin film rotating disk electrode method, the key technique used for evaluating nanocatalysts activity for ORR. To address these problems,I have carried out the following work in my ph. D theis:
1. ORR Methodology evaluation. Due to the low solubility of oxygen in the solution, the mass transport of02in both the solution phase and in the catalyst layer will affect the electrode reaction. At the same time, the internal resistance (IR) of solution will affect the estimation of the overpotential of the oxygen reduction reaction. To completely exclude the effects of the mass transfer and the uncompensated IR, is the prerequisite for deriving the intrinsic activity of nanocatalysts for ORR. After sysmtematic studies on the effects of the internal resistance of the solution on measurement of the oxygen reduction reaction, we have pointed out the method for correct IR compensation as well as misleading conclusions in the literature; By systematically varying the loading amount of the catalyst system, we have demonstrated the impact of mass transfer on evaluating catalysts activity for ORR. Some guidelines on how to rationally evaluate of nano-catalysts activity for ORR has been given.
2. Even for the best Pt based electrocatalyst for ORR, the overpotential at the onset is still above0.25V. In order to figure the origin for such high overpotential, we have systematically studied the the pH of the electrolyte solution on the thermodynamics and kinetics of OHad aodsorption.desorption as well on ORR kinetics. We found that OHad+H++e(?)H2O OHad+e(?)OH-, as parallel reaction occurs during ORR in the kinetic and kinetic and mass transport limited potential region, whose thermoelectrochemistry and kinetics strongly affect ORR kinetics. As the last step for ORR, the reversible desorption of OHad, one one hand its upper potential limit for its reversibility determines the onset potential for ORR, and its coverage determines the available sites for ORR. On the other hand, the net rate beteen the forward (OHad desorption) and backward reaction (H2O→OHad+H++e or OH→Had+e) determines the net rate for ORR. We have also prepared Ti supported PtxY catalysts with various pretreatment conditions and studied their ORR behavior, which confirms the above conclusions.
1.表征氧还原电催化剂活性的实验方法验证。由于溶液中,氧气的溶解度低,电极反应必然会受到溶液相以及催化剂层内传质的影响。同时,未补偿溶液电阻也会对估算的超电势带来影响。如何完全排除传质以及溶液内阻的影响,并获得电催化剂对氧还原反应的内在活性,是讨论氧还原催化剂的构、效关系的前提。本论文首先系统考察了溶液内阻对氧还原动力学测量的影响,并讨论了文献中有关论文在该问题上可能存在的误导,在此基础上提出了正确的溶液内阻补偿方法；然后系统地考察了催化剂的担载量,反应物在催化剂层中的传质对利用薄膜旋转圆盘电极技术获取氧还原动力学数据的影响,指出了正确利用该技术合理评价氧还原电极反应的内在活性的注意事项。
2.为了弄清铂基催化剂上氧还原的高超电势的起源,我们系统研究电解质溶液的pH值对Pt电极上H和OH的吸、脱附反应：尤其是OHad+H++e(?)H20(酸性介质)或者OHad+e(?)OH-(碱性介质)以及氧还原动力学的影响。我们发现i)在氧还原的动力学以及动力学与传质混合控制的电位区,上述反应即是氧电催化还原反应的最后一步,又是与氧还原平行进行、竞争反应活性位点的另一个可逆反应。而且,OHad的脱附动力学非常快,OHad的覆盖度主要受热力学因素决定；ⅱ)影响氧还原动力学的关键因素是在氧还原电位区与OH吸、脱附的热力学以及动力学。一方面,OH吸、脱附可逆发生的上限电位,决定了氧还原的起始电位,OHad的覆盖度限制了用于氧还原的活性位点数：另一方面,OHad脱附作为电催化氧还原反应的最后一步,而OHad+H++e(?)H2O或OHad+e(?)OH-在氧还原的动力学与传质混合控制的电位区可逆地向着两个方向同时进行,也限制了氧还原的净速度。在此基础上,我们还尝试制备了二元的PtxY催化剂,也证实了上述观点。
Proton exchange membrane fuel cells which can directly converted chemical energy into electrical energy near room temperature, and emit almost no or just a small amount of pollutants. Therefore, since the1960s, the R&D of such fuel cells has been greatly supported worldwide. However, by now such fuel cells have been successfully commercialized on large scale. Wherein an important bottleneck is that the kinetics for oxygen cathode reaction is very slow. Understanding the mechanism of the oxygen reduction reaction (ORR) has been one of the important research topic in the fuel cell catalysis, at the best Pt based electrocatalysts available so far, the overpotential at the onset for ORR is still as high as0.25V. After60years of research, much atomic, molecular level understanding for ORR has been gained. However, no consensus on ORR mechanism and key factors which limits ORR kinetics has been reached so far.This is probably due to, on one hand, ORR is a reaction involves4electron, multiple step complex process, on the other hand, some misunderstanding exists on using thin film rotating disk electrode method, the key technique used for evaluating nanocatalysts activity for ORR. To address these problems,I have carried out the following work in my ph. D theis:
1. ORR Methodology evaluation. Due to the low solubility of oxygen in the solution, the mass transport of02in both the solution phase and in the catalyst layer will affect the electrode reaction. At the same time, the internal resistance (IR) of solution will affect the estimation of the overpotential of the oxygen reduction reaction. To completely exclude the effects of the mass transfer and the uncompensated IR, is the prerequisite for deriving the intrinsic activity of nanocatalysts for ORR. After sysmtematic studies on the effects of the internal resistance of the solution on measurement of the oxygen reduction reaction, we have pointed out the method for correct IR compensation as well as misleading conclusions in the literature; By systematically varying the loading amount of the catalyst system, we have demonstrated the impact of mass transfer on evaluating catalysts activity for ORR. Some guidelines on how to rationally evaluate of nano-catalysts activity for ORR has been given.
2. Even for the best Pt based electrocatalyst for ORR, the overpotential at the onset is still above0.25V. In order to figure the origin for such high overpotential, we have systematically studied the the pH of the electrolyte solution on the thermodynamics and kinetics of OHad aodsorption.desorption as well on ORR kinetics. We found that OHad+H++e(?)H2O OHad+e(?)OH-, as parallel reaction occurs during ORR in the kinetic and kinetic and mass transport limited potential region, whose thermoelectrochemistry and kinetics strongly affect ORR kinetics. As the last step for ORR, the reversible desorption of OHad, one one hand its upper potential limit for its reversibility determines the onset potential for ORR, and its coverage determines the available sites for ORR. On the other hand, the net rate beteen the forward (OHad desorption) and backward reaction (H2O→OHad+H++e or OH→Had+e) determines the net rate for ORR. We have also prepared Ti supported PtxY catalysts with various pretreatment conditions and studied their ORR behavior, which confirms the above conclusions.
引文
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