燃料电池低铂载量膜电极制备新技术的探索及其研究
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摘要
质子交换膜燃料电池（PEMFC）因其比能量高、无污染、可快速低温启动等优点而受到人们的广泛关注。膜电极（MEA）是质子交换膜燃料电池的核心部件，不仅对燃料电池的性能有很大的影响，而且对降低其生产成本、加快其商业化进程具有很重要的现实意义。低温燃料电池大量使用贵金属铂作为催化剂的活性组分，成为燃料电池成本居高不下的重要因素，严重影响了低温燃料电池的商业化进程，因此，研究和开发具有低铂载量的膜电极，对于有效降低燃料电池的成本，促进燃料电池的发展和商业化进程具有十分重要的意义。
本文从降低燃料电池成本和提高其性能出发，采用原子层沉积、脉冲电沉积等新技术将活性组分直接沉积在扩散层上，探索制备了系列低铂载量膜电极，并对这些低铂载量膜电极的性能开展了研究。
采用原子层沉积法（ALD）直接在气体扩散层的XC-72R碳黑整平层上沉积铂活性组分，成功制备出了一种低铂载量膜电极。该膜电极的铂载量可低至0.26mg/cm2，在0.7V时电流密度可高达637mA/cm2。考察了该催化电极中的铂活性组分的形貌分布，电催化活性和稳定性以及由该催化电极制备成的膜电极的电池性能。结果表明：由于技术本身的限制，ALD方法制得的催化电极中铂活性组分的粒径高达8-10nm，尽管如此，该电极仍然显示了良好的电催化活性，其活性优于商业催化剂；在H2/O2单电池中，其最大功率密度高达3.34kW/gPt，是使用商业催化剂和传统方法制备膜电极的1.76倍，原因可能在于在ALD电极中，活性组分铂能够均匀地分布在电极表层，而由商业催化剂制备的电极具有一定的催化剂厚度层，相当大一部分铂都被包裹在电极的内层，影响了其催化效能的发挥。
使用经过预处理的碳纳米管（CNTs）替代XC-72R作为整平层碳材料，采用ALD技术成功制备出了一种高性能超低铂载量膜电极。与炭黑相比，纳米碳管具有更好的抗腐蚀能力；使用CNTs作为碳载体可以防止由于碳载体被腐蚀导致铂活性组分暴露而造成的电池性能下降，寿命减短的问题。结果显示：使用CNTs替代XC-72R的ALD法制备的催化电极中铂活性组分的粒径可由8-10nm降低为3-5nm；在铂载量低至0.26mg/cm2的情况下，ALD法制备出的膜电极的最大功率密度高达2.95kW/gPt，在通常的工作电压0.7V时的电流密度仍高达667mA/cm2,可完全媲美高铂载量商业催化剂制备的膜电极性能；此外，使用ALD法制备的基于CNTs的膜电极在400mA/cm2恒电流下持续放电100h后，其电压仍高达0.65V，衰减率为9.5%，而采用ALD法制备的基于XC-72R的膜电极放电100小时后的电压仅为0.62V，衰减率达16.2%，说明使用碳纳米管制备的ALD法膜电极具有更好的稳定性；这可能与碳纳米管具有更高的有序度、更好的抗氧化性能有关。交流阻抗和循环伏安测试说明这种低铂载量膜电极具有良好的电化学稳定性。
为了进一步考察碳载体对ALD法制备的膜电极性能的影响，我们还尝试采用XC-72取代XC-72R碳黑，制得了以XC-72碳黑为载体的高性能低铂载量的膜电极。实验结果表明：基于XC-72炭黑的ALD膜电极比起基于XC-72R以及CNTs的ALD膜电极具有更优异的性能。TEM显示基于XC-72的ALD法制备催化电极中铂活性组分分布均匀，粒径约为3-4nm；载量低至0.18mg/cm~2时其最大输出功率密度为4.80kW/gPt，分别是商业催化剂膜电极的2.5倍， XC-72R膜电极的1.43倍， CNTs膜电极的1.63倍；另外，在400mA/cm~2恒电流密度下持续放电100h后，ALD法制备的膜电极显示出优异的性能，电压仍高达0.74V，衰减率为1.8%，而商业催化剂制备的膜电极在运行100h后性能开始出现明显下降，衰减率为7.5%，ALD法制备的基于CNTs的膜电极衰减率为9.5%，基于XC-72R的膜电极衰减率为16.2%，证明该电极具有更高的铂利用率和稳定性；循环伏安测试说明这种低铂载量膜电极具有良好的电化学稳定性。关于为何XC-72碳黑作为基体载体制得的膜电极会出现更好的性能的原因及其机理，本文尚不能给出合理的解释，有待进一步的探索和研究。
本文探索的另一种新型的膜电极制备方法为脉冲电沉积法：采用脉冲电沉积法，在涂覆有整平层的碳纸的Ru/C+Nafion催化层上沉积铂活性组分，成功制备了一种基于Ru@Pt/C核壳结构催化剂的膜电极。该法可将铂活性组分直接沉积在电极的三相反应界面上，从而大大提高铂利用率。我们考察了Ru/C：Nafion比例、脉冲沉积电流密度以及沉积的铂载量对于膜电极的性能影响；实验结果表明在Ru/C：Nafion比例为2:1，脉冲沉积电流密度为0.5mA/cm~2，铂载量低至0.045mg/cm~2时能得到性能最优的膜电极；在氢气-空气燃料电池中，该膜电极在通常的工作电压0.7V时的电流密度仍高达336mA/cm~2，最大输出功率密度为0.56W/cm~2，而相同条件下测试的商业催化剂制备的膜电极的最大输出功率仅为0.40W/cm~2；TEM结果显示该法制备出的Ru@Pt/C核壳结构粒子大小约为~4.5nm。
本文还探索了使用微波合成法在涂覆有整平层的碳纸的炭黑层上沉积铂活性组分，制备了一种高性能低铂载量膜电极。实验结果表明：该法制备出的催化电极中铂活性组分高度分散，粒径均匀，约为2-3nm；考察了亲水层中碳载体含量和聚四氟乙烯（PTFE）含量对电池性能的影响，发现当碳载体含量为0.37mg/cm~2，PTFE含量为5%(by mass）时，膜电极性能最优，该膜电极铂载量可低至0.12mg/cm~2，在通常的工作电压0.7V时的电流密度仍高达538mA/cm~2，最大输出功率密度为0.89W/cm~2；交流阻抗和循环伏安测试说明这种低铂载量膜电极具有良好的电化学稳定性。
本文探索了三种制备低铂载量膜电极的新型制备技术，制备的膜电极均显示了优异的性能，尤其是原子层沉积技术和脉冲电沉积技术制备的膜电极，在质子交换膜燃料电池有很好的潜在应用前景。
Proton exchange membrane fuel cells (PEMFCs) have been acknowledged as one of themost promising alternative power sources due to their advantages, such as high power density,zero or low emission and quick startup at low temperature etc. As the key component ofPEMFC, membrane electrode assembly (MEA) has a great influence on both performanceand cost of fuel cell. At present, state-of-art carbon supported platinum is still the widely usedelectrocatalyst in MEA, which accounts for a large portion of PEMFC cost. To realize thecommercialization of PEMFC, lowering the platinum loading without loss of performance ofmembrane electrode assemblies has been one of the hottest topics in fuel cell field. In thisthesis, several novel techniques has been explored to be used for the preparation of MEAswith low Pt loading, and the performance of these MEAs, as well as the effect of preparationparameters on the performance have been extensively investigated.
Firstly, we prepared a high performance MEA with low Pt loading by using an atomiclayer deposition (ALD) technique. A cell performance of637mA/cm~2at0.7V was achievedwhen the platinum loading was lowered to0.26mg/cm~2. The morphology and distribution ofPt nanoparticles on the surface of the ALD-electrode was observed using a high-resolutiontransmission electron microscope (HR-TEM). The results revealed that although the activecomponent Pt on the ALD-electrode had a big particle size of8-10nm due to the limit ofALD technique, the electrode still showed superior activity to the electrode prepared withcommercial catalyst and conventional preparation method; The mass activity could be high upto3.34kW/gPt, which is1.76times higher than that of later. This improved mass activity canbe attributed to the well-dispersed Pt particles on the outer surface of the ALD-electrode; incontrast, most of the Pt nanoparticles in the electrode prepared with commercial catalyst andconventional preparation method were dispersed on the interior surface of the electrode,resulting in low Pt utilization.
Secondly, a high performance low platinum loadings MEA with carbon nanotubes(CNTs) instead of XC-72R was prepared by using ALD technique. It is well recognized thatCNTs has much better anti-corrosion properties than carbon black, using CNT as support canprevent the corrosion of support and the migration of platinum, resulting better performanceand durability. TEM images showed the Pt nanopaticles were highly dispersed on the CNTsbased ALD-electrode and had a particle size range of3-4nm, rather than8-10nm of theXC-72R based ALD-electrode. As the platinum loading was0.26mg/cm~2, the current density of the CNTs based ALD-MEA can reach as high as667mA/cm~2at0.7V of cell potential. Themass activity can reach4.80kW/gPt. In addition, this MEA showed excellent durability, after100h long term testing, no obvious performance change can be observed. The voltage of theCNTs based ALD-MEA reached0.65V, higher than that of XC-72R based ALD-MEA, and9.5%voltage loss compared with16.2%voltage loss of conventional MEA, confirming thehigh durability in ALD-MEA, and the superiority of CNTs substrate; This improvedperformance can be attributed to the higher order degree and better oxidation resistance ofCNTs. EIS and cyclic voltammetry (CV) test also reveal the good electrochemical stability ofCNTs based ALD-MEA.
To further investigate the effect of substrates supports on the performance of ALD-MEA,we prepare another ALD-MEA with by depositing Pt catalyst on the substrate layer of XC-72,It is found that the XC-72carbon black based MEA showed better performance comparedwith XC-72R and CNTs based MEAs. TEM images showed the Pt nanopaticles were highlydispersed on the XC-72based ALD-electrode and had a particle size range of3-4nm. Themass activity reached4.80kW/gPt with Pt loading of0.18mg/cm~2, which is2.53times higherthan that of the MEA prepared with commercial catalyst and conventional method, and,1.43times and1.63times higher than those of XC-72R based ALD-MEA and CNT basedALD-MEA, respectively. In100h of durability testing, the XC-72based ALD-MEAexhibited excellent durability,1.8%voltage loss when the MEA was discharged at a currentdensity of400mA/cm~2compared with7.5%,16.2%and9.5%voltage loss of conventionalMEA, XC-72R based ALD-MEA and CNT based ALD-MEA, respectively. Furthermore, thegood electrochemical stability is also confirmed by CV testing results. This article was not yetgiven a reasonable explanation of why XC-72R based ALD-MEA had better performance andfurther exploration and research were expected.
Another new technique we used for the preparation of MEA is pulse electrodeposition(PED) method; the MEA was prepared by electrodepositing Pt on the substrate prepared withRu/C catalyst, to form a Ru@Pt/C catalyst on the surface of the electrode. The effects of ratioof Ru/C to Nafion, deposition current density, and deposited Pt loading on the cellperformance were investigated. The optimal ratio of Ru/C to Nafion is ca.2:1, optimal pulsecurrent density is0.5mA/cm~2. The MEA prepared at optimal conditions and with Pt loadingof0.045mg/cm~2shows a performance of336mA/cm~2at0.7V, with the maximum outputpower of0.56W/cm~2in the H2/air fuel cell; The conventional MEA had a maximum outputpower of0.40W/cm~2with the same Pt loading. The particle size of Ru@Pt nanoparticle is~4.5nm by the TEM results.
Microwave synthesis technique has also been used for the preparation of MEA with lowPt loading. TEM images showed the Pt particles were highly dispersed in the electrode andthe particle size is in the range of2-3nm. The effects of loading amounts of carbon black andTeflon in the substrate layer on the cell performance were investigated. The optimal carbonblack loading is0.37mg/cm~2, and optimal Teflon loading is ca.5wt.%. The MEA preparedat optimal conditions and with Pt loading of0.12mg/cm~2at anode was prepared, in H2/O2single cell, it achieved current density of538mA/cm~2at0.7V with maximum power densityof0.89W/cm~2. Moreover, EIS and CV test provided strong clues for the goodelectrochemical stability of this low Pt loading MEA.
In summary, three types of new techniques has been explored to use for the preparationof low Pt loading MEA, all of them showed excellent activity and good stability, as well asgood durability. Especially, ALD and PED techniques may be the promising techniques forthe preparation of MEAs for PEM fuel cell applications.
本文从降低燃料电池成本和提高其性能出发，采用原子层沉积、脉冲电沉积等新技术将活性组分直接沉积在扩散层上，探索制备了系列低铂载量膜电极，并对这些低铂载量膜电极的性能开展了研究。
采用原子层沉积法（ALD）直接在气体扩散层的XC-72R碳黑整平层上沉积铂活性组分，成功制备出了一种低铂载量膜电极。该膜电极的铂载量可低至0.26mg/cm2，在0.7V时电流密度可高达637mA/cm2。考察了该催化电极中的铂活性组分的形貌分布，电催化活性和稳定性以及由该催化电极制备成的膜电极的电池性能。结果表明：由于技术本身的限制，ALD方法制得的催化电极中铂活性组分的粒径高达8-10nm，尽管如此，该电极仍然显示了良好的电催化活性，其活性优于商业催化剂；在H2/O2单电池中，其最大功率密度高达3.34kW/gPt，是使用商业催化剂和传统方法制备膜电极的1.76倍，原因可能在于在ALD电极中，活性组分铂能够均匀地分布在电极表层，而由商业催化剂制备的电极具有一定的催化剂厚度层，相当大一部分铂都被包裹在电极的内层，影响了其催化效能的发挥。
使用经过预处理的碳纳米管（CNTs）替代XC-72R作为整平层碳材料，采用ALD技术成功制备出了一种高性能超低铂载量膜电极。与炭黑相比，纳米碳管具有更好的抗腐蚀能力；使用CNTs作为碳载体可以防止由于碳载体被腐蚀导致铂活性组分暴露而造成的电池性能下降，寿命减短的问题。结果显示：使用CNTs替代XC-72R的ALD法制备的催化电极中铂活性组分的粒径可由8-10nm降低为3-5nm；在铂载量低至0.26mg/cm2的情况下，ALD法制备出的膜电极的最大功率密度高达2.95kW/gPt，在通常的工作电压0.7V时的电流密度仍高达667mA/cm2,可完全媲美高铂载量商业催化剂制备的膜电极性能；此外，使用ALD法制备的基于CNTs的膜电极在400mA/cm2恒电流下持续放电100h后，其电压仍高达0.65V，衰减率为9.5%，而采用ALD法制备的基于XC-72R的膜电极放电100小时后的电压仅为0.62V，衰减率达16.2%，说明使用碳纳米管制备的ALD法膜电极具有更好的稳定性；这可能与碳纳米管具有更高的有序度、更好的抗氧化性能有关。交流阻抗和循环伏安测试说明这种低铂载量膜电极具有良好的电化学稳定性。
为了进一步考察碳载体对ALD法制备的膜电极性能的影响，我们还尝试采用XC-72取代XC-72R碳黑，制得了以XC-72碳黑为载体的高性能低铂载量的膜电极。实验结果表明：基于XC-72炭黑的ALD膜电极比起基于XC-72R以及CNTs的ALD膜电极具有更优异的性能。TEM显示基于XC-72的ALD法制备催化电极中铂活性组分分布均匀，粒径约为3-4nm；载量低至0.18mg/cm~2时其最大输出功率密度为4.80kW/gPt，分别是商业催化剂膜电极的2.5倍， XC-72R膜电极的1.43倍， CNTs膜电极的1.63倍；另外，在400mA/cm~2恒电流密度下持续放电100h后，ALD法制备的膜电极显示出优异的性能，电压仍高达0.74V，衰减率为1.8%，而商业催化剂制备的膜电极在运行100h后性能开始出现明显下降，衰减率为7.5%，ALD法制备的基于CNTs的膜电极衰减率为9.5%，基于XC-72R的膜电极衰减率为16.2%，证明该电极具有更高的铂利用率和稳定性；循环伏安测试说明这种低铂载量膜电极具有良好的电化学稳定性。关于为何XC-72碳黑作为基体载体制得的膜电极会出现更好的性能的原因及其机理，本文尚不能给出合理的解释，有待进一步的探索和研究。
本文探索的另一种新型的膜电极制备方法为脉冲电沉积法：采用脉冲电沉积法，在涂覆有整平层的碳纸的Ru/C+Nafion催化层上沉积铂活性组分，成功制备了一种基于Ru@Pt/C核壳结构催化剂的膜电极。该法可将铂活性组分直接沉积在电极的三相反应界面上，从而大大提高铂利用率。我们考察了Ru/C：Nafion比例、脉冲沉积电流密度以及沉积的铂载量对于膜电极的性能影响；实验结果表明在Ru/C：Nafion比例为2:1，脉冲沉积电流密度为0.5mA/cm~2，铂载量低至0.045mg/cm~2时能得到性能最优的膜电极；在氢气-空气燃料电池中，该膜电极在通常的工作电压0.7V时的电流密度仍高达336mA/cm~2，最大输出功率密度为0.56W/cm~2，而相同条件下测试的商业催化剂制备的膜电极的最大输出功率仅为0.40W/cm~2；TEM结果显示该法制备出的Ru@Pt/C核壳结构粒子大小约为~4.5nm。
本文还探索了使用微波合成法在涂覆有整平层的碳纸的炭黑层上沉积铂活性组分，制备了一种高性能低铂载量膜电极。实验结果表明：该法制备出的催化电极中铂活性组分高度分散，粒径均匀，约为2-3nm；考察了亲水层中碳载体含量和聚四氟乙烯（PTFE）含量对电池性能的影响，发现当碳载体含量为0.37mg/cm~2，PTFE含量为5%(by mass）时，膜电极性能最优，该膜电极铂载量可低至0.12mg/cm~2，在通常的工作电压0.7V时的电流密度仍高达538mA/cm~2，最大输出功率密度为0.89W/cm~2；交流阻抗和循环伏安测试说明这种低铂载量膜电极具有良好的电化学稳定性。
本文探索了三种制备低铂载量膜电极的新型制备技术，制备的膜电极均显示了优异的性能，尤其是原子层沉积技术和脉冲电沉积技术制备的膜电极，在质子交换膜燃料电池有很好的潜在应用前景。
Proton exchange membrane fuel cells (PEMFCs) have been acknowledged as one of themost promising alternative power sources due to their advantages, such as high power density,zero or low emission and quick startup at low temperature etc. As the key component ofPEMFC, membrane electrode assembly (MEA) has a great influence on both performanceand cost of fuel cell. At present, state-of-art carbon supported platinum is still the widely usedelectrocatalyst in MEA, which accounts for a large portion of PEMFC cost. To realize thecommercialization of PEMFC, lowering the platinum loading without loss of performance ofmembrane electrode assemblies has been one of the hottest topics in fuel cell field. In thisthesis, several novel techniques has been explored to be used for the preparation of MEAswith low Pt loading, and the performance of these MEAs, as well as the effect of preparationparameters on the performance have been extensively investigated.
Firstly, we prepared a high performance MEA with low Pt loading by using an atomiclayer deposition (ALD) technique. A cell performance of637mA/cm~2at0.7V was achievedwhen the platinum loading was lowered to0.26mg/cm~2. The morphology and distribution ofPt nanoparticles on the surface of the ALD-electrode was observed using a high-resolutiontransmission electron microscope (HR-TEM). The results revealed that although the activecomponent Pt on the ALD-electrode had a big particle size of8-10nm due to the limit ofALD technique, the electrode still showed superior activity to the electrode prepared withcommercial catalyst and conventional preparation method; The mass activity could be high upto3.34kW/gPt, which is1.76times higher than that of later. This improved mass activity canbe attributed to the well-dispersed Pt particles on the outer surface of the ALD-electrode; incontrast, most of the Pt nanoparticles in the electrode prepared with commercial catalyst andconventional preparation method were dispersed on the interior surface of the electrode,resulting in low Pt utilization.
Secondly, a high performance low platinum loadings MEA with carbon nanotubes(CNTs) instead of XC-72R was prepared by using ALD technique. It is well recognized thatCNTs has much better anti-corrosion properties than carbon black, using CNT as support canprevent the corrosion of support and the migration of platinum, resulting better performanceand durability. TEM images showed the Pt nanopaticles were highly dispersed on the CNTsbased ALD-electrode and had a particle size range of3-4nm, rather than8-10nm of theXC-72R based ALD-electrode. As the platinum loading was0.26mg/cm~2, the current density of the CNTs based ALD-MEA can reach as high as667mA/cm~2at0.7V of cell potential. Themass activity can reach4.80kW/gPt. In addition, this MEA showed excellent durability, after100h long term testing, no obvious performance change can be observed. The voltage of theCNTs based ALD-MEA reached0.65V, higher than that of XC-72R based ALD-MEA, and9.5%voltage loss compared with16.2%voltage loss of conventional MEA, confirming thehigh durability in ALD-MEA, and the superiority of CNTs substrate; This improvedperformance can be attributed to the higher order degree and better oxidation resistance ofCNTs. EIS and cyclic voltammetry (CV) test also reveal the good electrochemical stability ofCNTs based ALD-MEA.
To further investigate the effect of substrates supports on the performance of ALD-MEA,we prepare another ALD-MEA with by depositing Pt catalyst on the substrate layer of XC-72,It is found that the XC-72carbon black based MEA showed better performance comparedwith XC-72R and CNTs based MEAs. TEM images showed the Pt nanopaticles were highlydispersed on the XC-72based ALD-electrode and had a particle size range of3-4nm. Themass activity reached4.80kW/gPt with Pt loading of0.18mg/cm~2, which is2.53times higherthan that of the MEA prepared with commercial catalyst and conventional method, and,1.43times and1.63times higher than those of XC-72R based ALD-MEA and CNT basedALD-MEA, respectively. In100h of durability testing, the XC-72based ALD-MEAexhibited excellent durability,1.8%voltage loss when the MEA was discharged at a currentdensity of400mA/cm~2compared with7.5%,16.2%and9.5%voltage loss of conventionalMEA, XC-72R based ALD-MEA and CNT based ALD-MEA, respectively. Furthermore, thegood electrochemical stability is also confirmed by CV testing results. This article was not yetgiven a reasonable explanation of why XC-72R based ALD-MEA had better performance andfurther exploration and research were expected.
Another new technique we used for the preparation of MEA is pulse electrodeposition(PED) method; the MEA was prepared by electrodepositing Pt on the substrate prepared withRu/C catalyst, to form a Ru@Pt/C catalyst on the surface of the electrode. The effects of ratioof Ru/C to Nafion, deposition current density, and deposited Pt loading on the cellperformance were investigated. The optimal ratio of Ru/C to Nafion is ca.2:1, optimal pulsecurrent density is0.5mA/cm~2. The MEA prepared at optimal conditions and with Pt loadingof0.045mg/cm~2shows a performance of336mA/cm~2at0.7V, with the maximum outputpower of0.56W/cm~2in the H2/air fuel cell; The conventional MEA had a maximum outputpower of0.40W/cm~2with the same Pt loading. The particle size of Ru@Pt nanoparticle is~4.5nm by the TEM results.
Microwave synthesis technique has also been used for the preparation of MEA with lowPt loading. TEM images showed the Pt particles were highly dispersed in the electrode andthe particle size is in the range of2-3nm. The effects of loading amounts of carbon black andTeflon in the substrate layer on the cell performance were investigated. The optimal carbonblack loading is0.37mg/cm~2, and optimal Teflon loading is ca.5wt.%. The MEA preparedat optimal conditions and with Pt loading of0.12mg/cm~2at anode was prepared, in H2/O2single cell, it achieved current density of538mA/cm~2at0.7V with maximum power densityof0.89W/cm~2. Moreover, EIS and CV test provided strong clues for the goodelectrochemical stability of this low Pt loading MEA.
In summary, three types of new techniques has been explored to use for the preparationof low Pt loading MEA, all of them showed excellent activity and good stability, as well asgood durability. Especially, ALD and PED techniques may be the promising techniques forthe preparation of MEAs for PEM fuel cell applications.
引文
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