中温固体氧化物燃料电池新型阳极材料的制备和性能表征
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摘要
固体氧化物燃料电池(SOFC)是一种高效的电化学能源转化器件。在商业化进程不断推进的情况下,传统的SOFC在运行中还存在着许多材料和技术方面的问题,其中两个主要的问题便是高催化活性材料的选择和材料使用过程中的稳定性。本文主要目的是在提高阳极在中温操作下的催化活性的同时获得高的稳定性。本论文工作分为三个部分,一部分研究了中温下一种新型的不含离子导电性的镍基陶瓷阳极,第二部分是构建复合阳极,对钙钛矿型阳极的成分进行优化,第三部分则是开发了一种新型的高催化性和稳定性的双钙钛矿阳极。
论文首先简单介绍了SOFC的操作原理和SOFC各关键材料,重点讨论了SOFC阳极材料的相关最新研究进展,在概述了SOFC的发展现状和趋势的基础上,确立了本论文的研究目标和研究内容。
第二章研究了一种镍基-镧系氧化物Ni-LnOx(Ln=La, Ce, Pr, Nd, Sm, Eu, Gd, Dy, Ho, Er, Yb, Tb)中温阳极。与传统的Ni-YSZ和Ni-SDC阳极不同的是,由于LnOx可忽略的离子导电性,这种阳极可认为是非离子导电的。这意味着该阳极的三相线界面(TPB)仅仅限于电解质/阳极的物理界面,从而导致阳极体内较低的TPB。即便如此,该阳极在中温下显示出了不低于Ni-SDC阳极的性能。在600℃湿氢气为燃料下Ni/LnOx(Sm, Eu, Ce, Gd, Dy, Ho, Er, Yb)阳极在SDC为电解质时对应的单电池的平均最高功率密度为600mW cm-2,高于Ni/SDC阳极对应的单电池的544mWcm-2。此外,以Ni-Sm2O3阳极为例,研究了这种阳极在ScSZ电解质下的电极性能。在700℃湿氢气为燃料时,Ni-Sm2O3阳极以ScSZ为电解质时对应的单电池最高功率密度为410mW cm-2,界面阻抗为0.7Ωcm2,与文献报道同电解质下以Ni-SDC或Ni-YSZ为阳极的单电池的功率密度处于同一水平。通过分析我们推测阳极的高性能可能来自于LnOx独特的氧化催化能力。
论文第三章本章接上一章,以Ni-LnOx (Ln=Dy, Ho, Er, Yb)阳极为例,较系统的研究了这种不含离子导电性的高性能阳极的催化机理。通过TPR的表征发现Ni粒子和镧系氧化物之间有很强的相互作用,Ni-LnOx相对纯Ni更多的耗氢量表明材料有多余的氢物种的吸附和迁移,而这种溢流效应可以增强阳极反应的速率,提高电极性能。通过测试电池在燃料不同氢分压时的阻抗谱比较进一步证实了Ni-LnOx阳极中氢物种溢流效应的存在。通过与Ni-SDC阳极的对比,我们可以推断,在阳极中催化活性和三相线长度的意义同等重要。然而,关于这种镍基镧系氧化物阳极催化氧化机理需要更深入的理论和实验的研究。
第四章采用机械混合法制备了SrFe1.5Mo0.5O6-δ-Sm0.8Ce0.2O1.9(SFM-SDC)复合阳极。采用氧渗透法测试了在氧化性和还原性气氛下SFM的氧离子电导率。基于SFM阳极较低的离子电导,向电极中添加了SDC第二相。考察了不同混合量的SDC对SFM基电极的电导率和微观结构的影响。采用电化学阻抗谱测量了以SFM-SDC为电极的对称电池,结果表明SFM-SDC电极的极化电阻(Rp)随SDC的加入而减小。单电池的测试表明,在30wt.%SDC时界面极化电阻得存在最小值(700℃时0.258Ωcm2)。阻抗谱的分析表明SDC提高电极性能的原因在于其高的离子电导率和高的催化活性。此外,SFM-SDC阳极在氧化还原循环测试和抗积碳测试中也表现出了良好的稳定性。
第五章考察了SrTi0.5Ni0.25Mo0.25O3作为SOFC阳极材料的可行性。XRD结果表明通过向SrNi0.5Mo0.5O3的B位掺杂50mo1.%的Ti可以使得材料在还原性气氛下结构稳定,而继续增大掺杂量则会造成材料的电导率的降低。测试得到SrTi0.5Ni0.25Mo0.25O3在600-800℃的温度范围间的总电导率为14-20S cm-1,满足SOFC对阳极材料电导率的基本要求。STNM在高温(1200℃)与电解质LSGM无明显的反应,且STNM的热膨胀系数约为12.8×10-6K-1,与LSGM的热膨胀系数十分接近。电化学测试表明以STNM为阳极,LSGM电解质支撑的单电池在800℃的最大输出功率为335mWcm-2,对应的极化阻抗为0.305Ω cm2。其电池功率输出与以(La0.75Sr0.25)0.9Cr0.5Mn0.5O3-δ为阳极的单电池处于同一水平。同时,STNM也表现出了对甲烷等碳氢化合物的良好的催化活性和稳定性。此外,采用第一性原理计算不同材料中的氧原子的P层电子中心,从中可以间接比较材料的氧催化活性的大小。基于上述研究结果,STNM是一种具有潜力的阳极材料,且通过成分的优化和微结构调整等工作还可以进一步提高电极性能。但此材料为阳极的电极反应机理还需要进一步研究。
Solid oxide fuel cells (SOFC) are electrochemical energy conversion devices with high efficiency. With the development of its commercialization implementation, there exist many issues for SOFCs so far that are material and technique problems, two of them are the choose of anode materials with high catalytic property as well as the stability of materials in use. The research of this thesis aims to improve the anode performance, mainly through:(1) developing a novel Ni based anode with negligible ionic conductivity,(2) improving the perovskite anode material by introducting an oxygen ion-conducting oxide,(3) developing new alternative double perovskite anode material.
At first, the SOFC principle and the key component materials were briefly introduced at first. Based on highlighting the present development status and direction for SOFCs, proposal on the thesis work was thus presented in this chapter.
In chapter2, Ni-LnOx (Ln=La, Ce, Pr, Nd, Sm, Eu, Gd, Dy, Ho, Er, Yb, Tb) composite anodes were developed for intermediate temperature SOFCs. Unlike the conventionalNi-YSZ and Ni-SDC anodes, this anode was considered to be non-ionic conductive due to the negligible ionic conductivity of LnOx. This meant TPB in the anode should be constricted to the physical interface between the electrolyte and anode so that the anode bulk possessed far small TPB. Even so, when the porosity was high enough to eliminate concentration polarization, the Ni-LnOx (Ln=Sm, Eu, Ce, Gd, Dy, Ho, Er and Yb) anodes exhibit very high performance; power density over600mW cm-2is achieved at600℃, comparable to, if not higher than those with the Ni-SDC anodes when the same cathodes and electrolytes were applied. In addition, Ni-Siri2O3cermets were investigated as the anodes with scandia-stabilized zirconia (ScSZ) electrolytes. Single cells with a Ni-SDC interlayer generated peak power density of410mW cm-2at700℃, and the interfacial polarization is about0.7Ω cm2. The high anode performance with both doped ceria electrolytes and stabilized zirconia electrolytes suggested that the high performance in Ni-LnOx (Ln=Sm, Eu, Ce, Gd, Dy, Ho, Er and Yb) anode was possibly due to the catalytic property of LnOx
In chapter3, taken Ni-LnOx (Ln=Dy, Ho, Er and Yb) cermet anodes as example, more systematic study had been carried out for this anode with negligible ionic conductivity. Temperature programmed reduction of NiO mixed with LnOx has shown that the surface properties of Ni in cermets are affected by the neighboring oxide panicles and that the interaction of NiO with LnOx is strong. High H2consumption implied that LnOx possessed high hydrogen adsoiption capability which might enhance spill-over process, thus promoting the surface diffusion with charge transfer through spillover reactions. The hydrogen spillover effect is further shown with impedance spectroscopy. It is reasonable to conclude that the catalytic behavior of LnOx with the promoting effect through nickel and LnOx coupling via the spillover reactions at the TPB is comparable to that of SDC by the extension of the three-phase boundary regions through oxide ion conduction. A continued concerted effort of theory and experiments is proposed in order to unambiguously elucidate the mechanism of the hydrogen oxidation reaction at these novel anodes.
In chapter4, Sr2Fe1.5Mo0.5O6-δ (SFM) perovskite was carefully investigated by modifying and optimizing the electrode microstructure. Its ionic conductivity under cathodic and anodic atmosphere was determined with oxygen permeation measurement. Sm0.8Ce0.2O1.9(SDC) was incorporated into SFM electrode to improve the anodic performance. A strong relation was observed between SDC addition and polarization losses, suggesting that the internal SFM-SDC contacts are active for H2oxidation. The best electrode performance was achieved for the composite with30wt.%SDC addition, resulting in an interfacial polarization resistance of0.258D cm2at700℃for La0.8Sr0.2Ga0.8Mg0.2O3-δ supported single cells. Electrochemical impedance spectroscopy analysis indicated that the high performance of SFM-SDC composite anodes was likely due to the high ionic conductivity and electro-catalytic activity of SDC by promoting the ionic exchange processes. Furthermore, this study had demonstrated that the SFM-SDC composite anodes were highly tolerant against redox cycling and carbon deposition.
In chapter5, SrTi0.5Ni0.25Mo0.25O3(STNM) was verified as a potential anode materials. STNM was comprehensively studied in terms of its chemical stability and thermal compatibility with La0.8Sr0.2Ga0.8Mg0.2O3-δ (LSGM) electrolytes, the electronic conductivity and electrochemical performance. The XRD results indicated that SrNi0.5Mo0.5O3was chemically stability with50mol%Ti doped. At600-S00℃the total conductivity of SrTi0.5Ni0.25Mo0.25O3(STNM) was14-20S cm-1, fulfilling the conductivity requirement of anode materials. The thermal expansion coefficient of STNM was closed to that of LSGM. The single cell with STNM anode, SLGM electrolyte and SSC cathode at800℃generated peak power density of335mW cm-2and the interfacial polarization resistance was0.305Ω cm2. It showed the performance not lower than that of the (La0.75Sr0.25)0.9Cr0.5Mn0.5O3-δ anode. Besides, STNM anode exhibited stability for directly use of hydrocarbons as the fuel to some extent. In addition, the bulk oxygen p-band center was calculated with first-principles-based in order to indirectly demonstrate the catalytic activity of oxygen reduced. The performance of STNM cathode is expected to be improved by optimizing the electrode microstructure. The electrode reaction mechanism of STNM needs be further investigated.
论文首先简单介绍了SOFC的操作原理和SOFC各关键材料,重点讨论了SOFC阳极材料的相关最新研究进展,在概述了SOFC的发展现状和趋势的基础上,确立了本论文的研究目标和研究内容。
第二章研究了一种镍基-镧系氧化物Ni-LnOx(Ln=La, Ce, Pr, Nd, Sm, Eu, Gd, Dy, Ho, Er, Yb, Tb)中温阳极。与传统的Ni-YSZ和Ni-SDC阳极不同的是,由于LnOx可忽略的离子导电性,这种阳极可认为是非离子导电的。这意味着该阳极的三相线界面(TPB)仅仅限于电解质/阳极的物理界面,从而导致阳极体内较低的TPB。即便如此,该阳极在中温下显示出了不低于Ni-SDC阳极的性能。在600℃湿氢气为燃料下Ni/LnOx(Sm, Eu, Ce, Gd, Dy, Ho, Er, Yb)阳极在SDC为电解质时对应的单电池的平均最高功率密度为600mW cm-2,高于Ni/SDC阳极对应的单电池的544mWcm-2。此外,以Ni-Sm2O3阳极为例,研究了这种阳极在ScSZ电解质下的电极性能。在700℃湿氢气为燃料时,Ni-Sm2O3阳极以ScSZ为电解质时对应的单电池最高功率密度为410mW cm-2,界面阻抗为0.7Ωcm2,与文献报道同电解质下以Ni-SDC或Ni-YSZ为阳极的单电池的功率密度处于同一水平。通过分析我们推测阳极的高性能可能来自于LnOx独特的氧化催化能力。
论文第三章本章接上一章,以Ni-LnOx (Ln=Dy, Ho, Er, Yb)阳极为例,较系统的研究了这种不含离子导电性的高性能阳极的催化机理。通过TPR的表征发现Ni粒子和镧系氧化物之间有很强的相互作用,Ni-LnOx相对纯Ni更多的耗氢量表明材料有多余的氢物种的吸附和迁移,而这种溢流效应可以增强阳极反应的速率,提高电极性能。通过测试电池在燃料不同氢分压时的阻抗谱比较进一步证实了Ni-LnOx阳极中氢物种溢流效应的存在。通过与Ni-SDC阳极的对比,我们可以推断,在阳极中催化活性和三相线长度的意义同等重要。然而,关于这种镍基镧系氧化物阳极催化氧化机理需要更深入的理论和实验的研究。
第四章采用机械混合法制备了SrFe1.5Mo0.5O6-δ-Sm0.8Ce0.2O1.9(SFM-SDC)复合阳极。采用氧渗透法测试了在氧化性和还原性气氛下SFM的氧离子电导率。基于SFM阳极较低的离子电导,向电极中添加了SDC第二相。考察了不同混合量的SDC对SFM基电极的电导率和微观结构的影响。采用电化学阻抗谱测量了以SFM-SDC为电极的对称电池,结果表明SFM-SDC电极的极化电阻(Rp)随SDC的加入而减小。单电池的测试表明,在30wt.%SDC时界面极化电阻得存在最小值(700℃时0.258Ωcm2)。阻抗谱的分析表明SDC提高电极性能的原因在于其高的离子电导率和高的催化活性。此外,SFM-SDC阳极在氧化还原循环测试和抗积碳测试中也表现出了良好的稳定性。
第五章考察了SrTi0.5Ni0.25Mo0.25O3作为SOFC阳极材料的可行性。XRD结果表明通过向SrNi0.5Mo0.5O3的B位掺杂50mo1.%的Ti可以使得材料在还原性气氛下结构稳定,而继续增大掺杂量则会造成材料的电导率的降低。测试得到SrTi0.5Ni0.25Mo0.25O3在600-800℃的温度范围间的总电导率为14-20S cm-1,满足SOFC对阳极材料电导率的基本要求。STNM在高温(1200℃)与电解质LSGM无明显的反应,且STNM的热膨胀系数约为12.8×10-6K-1,与LSGM的热膨胀系数十分接近。电化学测试表明以STNM为阳极,LSGM电解质支撑的单电池在800℃的最大输出功率为335mWcm-2,对应的极化阻抗为0.305Ω cm2。其电池功率输出与以(La0.75Sr0.25)0.9Cr0.5Mn0.5O3-δ为阳极的单电池处于同一水平。同时,STNM也表现出了对甲烷等碳氢化合物的良好的催化活性和稳定性。此外,采用第一性原理计算不同材料中的氧原子的P层电子中心,从中可以间接比较材料的氧催化活性的大小。基于上述研究结果,STNM是一种具有潜力的阳极材料,且通过成分的优化和微结构调整等工作还可以进一步提高电极性能。但此材料为阳极的电极反应机理还需要进一步研究。
Solid oxide fuel cells (SOFC) are electrochemical energy conversion devices with high efficiency. With the development of its commercialization implementation, there exist many issues for SOFCs so far that are material and technique problems, two of them are the choose of anode materials with high catalytic property as well as the stability of materials in use. The research of this thesis aims to improve the anode performance, mainly through:(1) developing a novel Ni based anode with negligible ionic conductivity,(2) improving the perovskite anode material by introducting an oxygen ion-conducting oxide,(3) developing new alternative double perovskite anode material.
At first, the SOFC principle and the key component materials were briefly introduced at first. Based on highlighting the present development status and direction for SOFCs, proposal on the thesis work was thus presented in this chapter.
In chapter2, Ni-LnOx (Ln=La, Ce, Pr, Nd, Sm, Eu, Gd, Dy, Ho, Er, Yb, Tb) composite anodes were developed for intermediate temperature SOFCs. Unlike the conventionalNi-YSZ and Ni-SDC anodes, this anode was considered to be non-ionic conductive due to the negligible ionic conductivity of LnOx. This meant TPB in the anode should be constricted to the physical interface between the electrolyte and anode so that the anode bulk possessed far small TPB. Even so, when the porosity was high enough to eliminate concentration polarization, the Ni-LnOx (Ln=Sm, Eu, Ce, Gd, Dy, Ho, Er and Yb) anodes exhibit very high performance; power density over600mW cm-2is achieved at600℃, comparable to, if not higher than those with the Ni-SDC anodes when the same cathodes and electrolytes were applied. In addition, Ni-Siri2O3cermets were investigated as the anodes with scandia-stabilized zirconia (ScSZ) electrolytes. Single cells with a Ni-SDC interlayer generated peak power density of410mW cm-2at700℃, and the interfacial polarization is about0.7Ω cm2. The high anode performance with both doped ceria electrolytes and stabilized zirconia electrolytes suggested that the high performance in Ni-LnOx (Ln=Sm, Eu, Ce, Gd, Dy, Ho, Er and Yb) anode was possibly due to the catalytic property of LnOx
In chapter3, taken Ni-LnOx (Ln=Dy, Ho, Er and Yb) cermet anodes as example, more systematic study had been carried out for this anode with negligible ionic conductivity. Temperature programmed reduction of NiO mixed with LnOx has shown that the surface properties of Ni in cermets are affected by the neighboring oxide panicles and that the interaction of NiO with LnOx is strong. High H2consumption implied that LnOx possessed high hydrogen adsoiption capability which might enhance spill-over process, thus promoting the surface diffusion with charge transfer through spillover reactions. The hydrogen spillover effect is further shown with impedance spectroscopy. It is reasonable to conclude that the catalytic behavior of LnOx with the promoting effect through nickel and LnOx coupling via the spillover reactions at the TPB is comparable to that of SDC by the extension of the three-phase boundary regions through oxide ion conduction. A continued concerted effort of theory and experiments is proposed in order to unambiguously elucidate the mechanism of the hydrogen oxidation reaction at these novel anodes.
In chapter4, Sr2Fe1.5Mo0.5O6-δ (SFM) perovskite was carefully investigated by modifying and optimizing the electrode microstructure. Its ionic conductivity under cathodic and anodic atmosphere was determined with oxygen permeation measurement. Sm0.8Ce0.2O1.9(SDC) was incorporated into SFM electrode to improve the anodic performance. A strong relation was observed between SDC addition and polarization losses, suggesting that the internal SFM-SDC contacts are active for H2oxidation. The best electrode performance was achieved for the composite with30wt.%SDC addition, resulting in an interfacial polarization resistance of0.258D cm2at700℃for La0.8Sr0.2Ga0.8Mg0.2O3-δ supported single cells. Electrochemical impedance spectroscopy analysis indicated that the high performance of SFM-SDC composite anodes was likely due to the high ionic conductivity and electro-catalytic activity of SDC by promoting the ionic exchange processes. Furthermore, this study had demonstrated that the SFM-SDC composite anodes were highly tolerant against redox cycling and carbon deposition.
In chapter5, SrTi0.5Ni0.25Mo0.25O3(STNM) was verified as a potential anode materials. STNM was comprehensively studied in terms of its chemical stability and thermal compatibility with La0.8Sr0.2Ga0.8Mg0.2O3-δ (LSGM) electrolytes, the electronic conductivity and electrochemical performance. The XRD results indicated that SrNi0.5Mo0.5O3was chemically stability with50mol%Ti doped. At600-S00℃the total conductivity of SrTi0.5Ni0.25Mo0.25O3(STNM) was14-20S cm-1, fulfilling the conductivity requirement of anode materials. The thermal expansion coefficient of STNM was closed to that of LSGM. The single cell with STNM anode, SLGM electrolyte and SSC cathode at800℃generated peak power density of335mW cm-2and the interfacial polarization resistance was0.305Ω cm2. It showed the performance not lower than that of the (La0.75Sr0.25)0.9Cr0.5Mn0.5O3-δ anode. Besides, STNM anode exhibited stability for directly use of hydrocarbons as the fuel to some extent. In addition, the bulk oxygen p-band center was calculated with first-principles-based in order to indirectly demonstrate the catalytic activity of oxygen reduced. The performance of STNM cathode is expected to be improved by optimizing the electrode microstructure. The electrode reaction mechanism of STNM needs be further investigated.
引文
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