A_2BO_4（B=Cu，Mn）型复合氧化物的电化学性质研究
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摘要
固体氧化物燃料电池(SOFC)由于具有能量转换率高、燃料可选范围广、不需用贵金属催化剂以及全固态结构带来的操作方便等优点而被认为是一种很有发展前途的燃料电池。目前,降低操作温度,开发中低温(500～800oC)固体氧化物燃料电池成为SOFC发展方向。但操作温度降低,电极的极化损失增加,因此开发中低温高性能电极材料具有重要意义。A2BO4型复合氧化物具有合适的热膨胀系数,能较好地与CGO、LSGM等中温SOFC的电解质材料相匹配,在600～800 oC的中温范围内具有比LSCF体系更优良的氧表面交换性能和氧离子迁移能力,很有希望成为中温SOFC的新型阴极材料。
本论文采用甘氨酸-硝酸盐法合成了A2BO4型Cu系复合氧化物Ln2-xCexCuO4(Ln=La,Nd,Sm)阴极材料。利用XRD对其物相及热化学稳定性进行了表征。结果表明Ce在La2CuO4中的最大固溶度低于3%,而在Nd2CuO4和Sm2CuO4中的最大固溶度为20%。Ln2-xCexCuO4与电解质材料CGO在1100 oC空气气氛下进行混合烧结,未生成杂相,表现出良好的化学稳定性。考察了电极烧结温度对电极的微观结构和电化学性能的影响,发现在1000oC空气中烧结得到的电极与CGO电解质可形成良好的接触界面,电极表面形成均匀的多孔结构,粒子之间相互连接紧密。Ce4+离子的掺杂提高材料的电导率,Nd2-xCexCuO4和Sm2-xCexCuO4材料在中温区(500～750 oC)空气气氛下的电导率均超过60 S/cm。对阴极极化性能的研究结果表明,Sm2-xCexCuO4体系具有较高的阴极催化活性。其中当Ce掺杂量为0.2时,电极Sm1.8Ce0.2CuO4的极化电阻最小,750oC的极化电阻为0.37Ω.cm2。利用在不同氧分压条件下测试阴极的电化学性能来研究电极反应的动力学过程,从而确定电极反应速率控制步骤。由不同温度下极化电阻与氧分压的关系发现,Sm1.8Ce0.2CuO4电极反应主要存在三个过程,氧离子从TPB界面向电解质的转移过程、电极上发生的电荷转移过程以及氧的解离与吸附过程,其中电极反应速率控制步骤为电极上发生的电荷转移反应。
在Cu系阴极材料中选择性能最好的Sm1.8Ce0.2CuO4(SCC)材料,进行了SCC-CGO和SCC-Ag复合阴极性能的研究,以期进一步提高阴极性能。系统地考察了CGO和Ag复合量对电极电化学性能的影响。结果表明,CGO含量为5%的复合电极性能最好,750oC的极化电阻为0.17Ω.cm2。CGO的掺入有效地改善了电极和电解质的结合程度,降低了界面极化电阻。同时,阴极极化现象也得到了较大改善,750oC时,极化过电位为30 mV时的电流密度约为150 mA.cm-2。Ag的加入同样提高了电极的电化学性能,当Ag掺杂量为5%时,电极极化电阻最小。空气中750oC测试得到复合电极的极化电阻约为0.18Ω.cm2。
本文进一步制备并研究了Mn系A2BO4型阴极材料的电化学性能,考察了材料组成对其电化学性能的影响。结果表明,该材料在1100oC空气中与CGO电解质具有良好的化学相容性。A位阳离子缺位型Mn系氧化物具有较好的阴极性能。Sr1.5La0.35MnO4阴极在750 oC的极化电阻最小,为0.25Ω. cm2,这一数值与A位整比型的Sr2-xLaxMnO4阴极材料相比有了较大的降低。电极反应机理研究表明,在不同的温度和氧分压下,电极反应有着不同的速率控制步骤。
Solid Oxide Fuel Cells (SOFC) was considered as a promising fuel cell because of its higher energy efficiency, rapid electrode kinetics without using expensive electrocatalysts such as Pt, the possibility of processing CO, CH4 and other Carbon based fuels, and flexibility to stacks of cells. Intermediate Temperature Solid Oxide Fuel Cells (IT-SOFCs) become a leading trend for development of SOFC. However, lowering the temperature leads to the increasing of electrode polarization loss. So it is important to research and explore electrode materials with high performance to meet the requirement of IT-SOFCs. A2BO4 type oxide materials exhibited suitable thermal expansion coefficient (TEC), which can match reasonably well with the CGO or LSGM electrolyte materials. And in the temperature range of 600～800oC, this material showed higher oxygen diffusion and surface exchange coefficients than the traditional LSCF system. All these results imply that A2BO4 type oxide is a kind of promising cathode materials for IT-SOFCs.
In this thesis, cathode materials Ln2-xCexCuO4(Ln=La,Nd,Sm) for IT-SOFCs were prepared by glycine-nitrate process (GNP). The chemical compatibility of the electrode and electrolyte at high temperature and effects of the sintering temperature on the microstructure and electrochemical properties were investigated, respectively. The results showed that maximum solubility of Ce in the La2-xCexCuO4 is 3% and the maximum solubility of Ce in the Nd2-xCexCuO4 and Sm2-xCexCuO4 is 20%. The electrode materials and the electrolyte CGO have good chemical compatibility at 1050 oC. The microstructure of the electrode sintered at 1000oC showed a structure with reasonable porosity and well-necked particles. The good adhesion between electrode and electrolyte is also observed. The doping of Ce increased the conductivity of these materials. The conductivities of Nd2-xCexCuO4 and Sm2-xCexCuO4 exceed 60 S/cm in the intermediate temperature range of 500～750oC. Sm2-xCexCuO4 system exhibited the highest performance. When the doping content of Ce is 20%, the electrode gave the lowest polarization resistance (0.37Ω.cm2) at 750 oC in air. Oxygen partial pressure effect experiments have been performed to study the mechanism of the reaction occurred on the electrode. We have studied variations of the electrode polarization resistance with temperatures and oxygen partial pressures, respectively. The results showed that the possible rate limiting step for cathode reaction depends on the charge transfer process, oxygen adsorption-desorption process and oxygen ion transfer from the TPB to the CGO electrolyte process. The rate limiting step for Sm1.8Ce0.2CuO4 cathode is the charge transfer process.
In order to improve the electrode property further, the composite cathode of Sm1.8Ce0.2CuO4-CGO (SCC-CGO) and Sm1.8Ce0.2CuO4-Ag (SCC-Ag) electrodes were studied systematically. The results showed that the addition of CGO powders into SCC electrode was effective in improving the electrode performance and the bonding of the electrode and electrolyte. The addition of 5 wt.% CGO in SCC resulted in the lowest polarization resistance of 0.17 ?.cm2 at 750 oC in air. And the polarization phenomenon of the cathode was improved simultaneously. When the current density reached 150 mA.cm-2, the over-potential is 30 mV at 750 oC in air. The SCC-Ag composite cathode also showed fine electrochemical performance. The addition of 5 wt.% Ag in SCC resulted in the lowest polarization resistance of 0.18 ?.cm2 at 750 oC in air.
Besides, the A2BO4 type manganate cathode materials, Sr2-xLaxMnO4 and Sr1.5LaxMnO4, were also prepared. The electrochemical properties of these materials were studied as used for SOFC cathode. The results showed that Sr1.5LaxMnO4 cathode exhibited improved performance. The lowest polarization resistance (0.25 ?.cm2) was obtained for Sr1.5La0.35MnO4 at 750 oC in air. Study on the oxygen reduction mechanism of Sr1.5La0.35MnO4 electrode showed that the rate limiting step changed with the variation of temperature and PO2.
本论文采用甘氨酸-硝酸盐法合成了A2BO4型Cu系复合氧化物Ln2-xCexCuO4(Ln=La,Nd,Sm)阴极材料。利用XRD对其物相及热化学稳定性进行了表征。结果表明Ce在La2CuO4中的最大固溶度低于3%,而在Nd2CuO4和Sm2CuO4中的最大固溶度为20%。Ln2-xCexCuO4与电解质材料CGO在1100 oC空气气氛下进行混合烧结,未生成杂相,表现出良好的化学稳定性。考察了电极烧结温度对电极的微观结构和电化学性能的影响,发现在1000oC空气中烧结得到的电极与CGO电解质可形成良好的接触界面,电极表面形成均匀的多孔结构,粒子之间相互连接紧密。Ce4+离子的掺杂提高材料的电导率,Nd2-xCexCuO4和Sm2-xCexCuO4材料在中温区(500～750 oC)空气气氛下的电导率均超过60 S/cm。对阴极极化性能的研究结果表明,Sm2-xCexCuO4体系具有较高的阴极催化活性。其中当Ce掺杂量为0.2时,电极Sm1.8Ce0.2CuO4的极化电阻最小,750oC的极化电阻为0.37Ω.cm2。利用在不同氧分压条件下测试阴极的电化学性能来研究电极反应的动力学过程,从而确定电极反应速率控制步骤。由不同温度下极化电阻与氧分压的关系发现,Sm1.8Ce0.2CuO4电极反应主要存在三个过程,氧离子从TPB界面向电解质的转移过程、电极上发生的电荷转移过程以及氧的解离与吸附过程,其中电极反应速率控制步骤为电极上发生的电荷转移反应。
在Cu系阴极材料中选择性能最好的Sm1.8Ce0.2CuO4(SCC)材料,进行了SCC-CGO和SCC-Ag复合阴极性能的研究,以期进一步提高阴极性能。系统地考察了CGO和Ag复合量对电极电化学性能的影响。结果表明,CGO含量为5%的复合电极性能最好,750oC的极化电阻为0.17Ω.cm2。CGO的掺入有效地改善了电极和电解质的结合程度,降低了界面极化电阻。同时,阴极极化现象也得到了较大改善,750oC时,极化过电位为30 mV时的电流密度约为150 mA.cm-2。Ag的加入同样提高了电极的电化学性能,当Ag掺杂量为5%时,电极极化电阻最小。空气中750oC测试得到复合电极的极化电阻约为0.18Ω.cm2。
本文进一步制备并研究了Mn系A2BO4型阴极材料的电化学性能,考察了材料组成对其电化学性能的影响。结果表明,该材料在1100oC空气中与CGO电解质具有良好的化学相容性。A位阳离子缺位型Mn系氧化物具有较好的阴极性能。Sr1.5La0.35MnO4阴极在750 oC的极化电阻最小,为0.25Ω. cm2,这一数值与A位整比型的Sr2-xLaxMnO4阴极材料相比有了较大的降低。电极反应机理研究表明,在不同的温度和氧分压下,电极反应有着不同的速率控制步骤。
Solid Oxide Fuel Cells (SOFC) was considered as a promising fuel cell because of its higher energy efficiency, rapid electrode kinetics without using expensive electrocatalysts such as Pt, the possibility of processing CO, CH4 and other Carbon based fuels, and flexibility to stacks of cells. Intermediate Temperature Solid Oxide Fuel Cells (IT-SOFCs) become a leading trend for development of SOFC. However, lowering the temperature leads to the increasing of electrode polarization loss. So it is important to research and explore electrode materials with high performance to meet the requirement of IT-SOFCs. A2BO4 type oxide materials exhibited suitable thermal expansion coefficient (TEC), which can match reasonably well with the CGO or LSGM electrolyte materials. And in the temperature range of 600～800oC, this material showed higher oxygen diffusion and surface exchange coefficients than the traditional LSCF system. All these results imply that A2BO4 type oxide is a kind of promising cathode materials for IT-SOFCs.
In this thesis, cathode materials Ln2-xCexCuO4(Ln=La,Nd,Sm) for IT-SOFCs were prepared by glycine-nitrate process (GNP). The chemical compatibility of the electrode and electrolyte at high temperature and effects of the sintering temperature on the microstructure and electrochemical properties were investigated, respectively. The results showed that maximum solubility of Ce in the La2-xCexCuO4 is 3% and the maximum solubility of Ce in the Nd2-xCexCuO4 and Sm2-xCexCuO4 is 20%. The electrode materials and the electrolyte CGO have good chemical compatibility at 1050 oC. The microstructure of the electrode sintered at 1000oC showed a structure with reasonable porosity and well-necked particles. The good adhesion between electrode and electrolyte is also observed. The doping of Ce increased the conductivity of these materials. The conductivities of Nd2-xCexCuO4 and Sm2-xCexCuO4 exceed 60 S/cm in the intermediate temperature range of 500～750oC. Sm2-xCexCuO4 system exhibited the highest performance. When the doping content of Ce is 20%, the electrode gave the lowest polarization resistance (0.37Ω.cm2) at 750 oC in air. Oxygen partial pressure effect experiments have been performed to study the mechanism of the reaction occurred on the electrode. We have studied variations of the electrode polarization resistance with temperatures and oxygen partial pressures, respectively. The results showed that the possible rate limiting step for cathode reaction depends on the charge transfer process, oxygen adsorption-desorption process and oxygen ion transfer from the TPB to the CGO electrolyte process. The rate limiting step for Sm1.8Ce0.2CuO4 cathode is the charge transfer process.
In order to improve the electrode property further, the composite cathode of Sm1.8Ce0.2CuO4-CGO (SCC-CGO) and Sm1.8Ce0.2CuO4-Ag (SCC-Ag) electrodes were studied systematically. The results showed that the addition of CGO powders into SCC electrode was effective in improving the electrode performance and the bonding of the electrode and electrolyte. The addition of 5 wt.% CGO in SCC resulted in the lowest polarization resistance of 0.17 ?.cm2 at 750 oC in air. And the polarization phenomenon of the cathode was improved simultaneously. When the current density reached 150 mA.cm-2, the over-potential is 30 mV at 750 oC in air. The SCC-Ag composite cathode also showed fine electrochemical performance. The addition of 5 wt.% Ag in SCC resulted in the lowest polarization resistance of 0.18 ?.cm2 at 750 oC in air.
Besides, the A2BO4 type manganate cathode materials, Sr2-xLaxMnO4 and Sr1.5LaxMnO4, were also prepared. The electrochemical properties of these materials were studied as used for SOFC cathode. The results showed that Sr1.5LaxMnO4 cathode exhibited improved performance. The lowest polarization resistance (0.25 ?.cm2) was obtained for Sr1.5La0.35MnO4 at 750 oC in air. Study on the oxygen reduction mechanism of Sr1.5La0.35MnO4 electrode showed that the rate limiting step changed with the variation of temperature and PO2.
引文
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