固体氧化物燃料电池电解质材料的制备与性能研究
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摘要
固体氧化物燃料电池(SOFC)是直接将燃料和氧化剂的化学能转换为电能的全固态能量装置。目前SOFC体系中广泛使用的电解质材料为钇稳定的氧化锆(YSZ)。但其要求必须在较高的工作温度(900－1000℃)下才具有足够高的离子电导率,而这将引起电池组件之间的化学反应、电极烧结、热膨胀系数不匹配等问题。本文以立方萤石结构的Ce0.8Sm0.2O1.9基电解质材料和六方磷灰石型晶体结构的La9.33Si16O26电解质材料为研究对象,研究了掺杂和复合手段对电解质材料导电性能的影响,主要开展了以下几方面的工作。
(1)利用化学共沉淀法合成了Ce_(0.8)Sm_(0.2-x)Y_xO_(1.9) (x=0,0.05,0.1,0.15)粉体材料,经传统烧结工艺制备出了陶瓷烧结块体材料。以XRD、SEM和交流阻抗等分析测试手段对电解质材料的微观结构和性能进行了表征；对Y~(3+)掺杂量对Ce_(0.8)Sm_(0.2-x)Y_xO_(1.9)电解质材料的导电性能的影响进行了研究。结果表明,随Y~(3+)掺杂量的增加,电解质的电导率呈现先增大后减小的趋势,x=0.1时达到最大,700℃时总电导率为7.94×10-3S/cm；初步探讨了Ce_(0.8)Sm_(0.2-x)Y_xO_(1.9)电解质材料的导电机理；
(2)采用化学共沉淀法制备出了5x (x=0,0.2,0.4)粉体材料,经传统烧结制度获得了陶瓷烧结块体材料；以XRD和交流阻抗等分析测试手段对电解质材料的微观结构和性能进行了表征；对La~(3+)的含量对其导电性能的影响进行了研究。结果表明,过量La~(3+)的加入能够很大程度的提高电解质材料的离子电导率,从x=0到x=0.4,电导率从2.5×10-4 S·cm~(-1)提高至1.48×10-3S·cm~(-1),提高了约6倍；利用Jonscher经验公式对其导电过程机理进行了初步探讨,认为长程导电机制在该种电解质材料的导电过程中占主导地位。
(3)采用复合技术制备出了复合氧离子导电体；分别利用共沉淀法、溶剂热法和球磨等方法引入第二相制备出了具有不同复合量的Ce_(0.8)Sm_(0.2)0_(1.9)-La_(9.33)Si_6O_(26)复合电解质材料；采用传统的烧结工艺过程获得了相应的烧结块体复合电解质陶瓷材料；利用XRD、SEM、EDS和交流阻抗技术等检测手段对其物相组成和导电性能进行了表征。研究发现经复合后形成了由Ce0.8Sm0.2O1.9和La_(9.33)Si_6O_(26)两种物相所组成的复合材料体系；认为在复合电解质的导电过程中,两相间的界面效应对于总电导率的提高有着重要的作用；探讨了第二相的复合量和引入手段对于复合电解质导电性能的影响。
(4)利用两步共沉淀法合成了Ce0.8Sm0.1Y0.1O1.9-La9.73Si6O26.6复合电解质材料,利用交流阻抗分析技术对其导电性能进行了测试,结果表明,复合相的相纯度以及界面处固溶反应的发生对于复合电解质的导电性能具有重要影响。
Solid oxide fuel cell (SOFC) is an all-solid-state energy device which could convert directly the chemical energy of fuels and oxidants into electrical energy. At present the most electrolyte materials used in the SOFC system are yttrium stable zirconia (YSZ). YSZ requires a high operating temperature (900-1000℃) to get high enough ionic conductivity, and this will cause problems such as the chemical reaction of battery components, electrode sintering and thermal expansion coefficient mismatch. Ce0.8Sm0.2O1.9-based electrolytes with a fluorite structure and La_(9.33)Si_6O_(26)-based electrolytes with an apatite structure were studied in this thesis. Influences of doping and composite technology on the conductive properties of these two electrolyte materials were studied. The research work comprises the following aspects.
(1) Chemical co-precipitation method was employed to synthesize the Ce_(0.8)Sm_(0.2-x)Y_xO_(1.9)(x=0,0.05,0.1,0.15) powers and the conventional sintering technique was utilized to prepare the related ceramics. The structure and electrical properties of the electrolyte materials were characterized by XRD, SEM and ac impedance technology, respectively. The influence of Y~(3+) contents on the electrical properties of Ce_(0.8)Sm_(0.2-x)Y_xO_(1.9) ceramics was studied. With Y~(3+) content increases, electrical conductivities of electrolytes increase first and then decrease and reach a maximum value when x=0.1, the total conductivity is 7.94×10-3 S·cm~(-1) at 700℃. The conductive mechanism was discussed preliminary.
(2) Chemical co-precipitation method was employed to synthesize the La9.3~(3+)xSi6O26+1.5x (x=0,0.2,0.4) powers and the conventional sintering technique was utilized to prepare the related ceramics. The structure and electrical properties of the electrolyte materials were characterized by XRD and ac impedance technology. The influence of La~(3+) contents on the electrical properties of La9.3~(3+)xSi6O26+1.5x ceramics was studied. Addition of excessive La~(3+) could enhance obviously electrical conductivities of electrolytes. From x=0 to x=0.4, conductivities increase from 2.5×10-4Scm~(-1)to 1.48×10-3S·cm~(-1) at 700℃, about 6 times improved. The conductive mechanism was discussed with Jonscher experience formula, and long-range conduction mechanism was regarded as the dominant one.
(3) Ce0.8Sm0.201.9-La9.33Si6026.6 composite oxygen ion conductors were prepared by composite technology. The second phase was introduced via chemical co-precipitation, solvothermal and ball milling mixing. The composite electrolyte materials with different composite amounts were prepared. The conventional sintering technique was utilized to prepare the related ceramics. The phase and electrical properties of the electrolyte materials were characterized by XRD, SEM, EDS and ac impedance technology. The results show that composite electrolytes consist of Ce0.8Sm0.2O19 and La9.33Si6026-Interfaces between phases play important role in total conductivities. The influences of quantity and introducing way of the second phase on the composites conductive properties were studied.
(4) Ce0.8Sm0.1Y0.1O1.9-La9.73Si6026 composite electrolyte was prepared by two-step co-precipitation method. The electrical properties were characterized by ac impedance technology. The results showed that phase purity and solid solution reaction between interfaces have important influences on the performances of composite electrolytes.
(1)利用化学共沉淀法合成了Ce_(0.8)Sm_(0.2-x)Y_xO_(1.9) (x=0,0.05,0.1,0.15)粉体材料,经传统烧结工艺制备出了陶瓷烧结块体材料。以XRD、SEM和交流阻抗等分析测试手段对电解质材料的微观结构和性能进行了表征；对Y~(3+)掺杂量对Ce_(0.8)Sm_(0.2-x)Y_xO_(1.9)电解质材料的导电性能的影响进行了研究。结果表明,随Y~(3+)掺杂量的增加,电解质的电导率呈现先增大后减小的趋势,x=0.1时达到最大,700℃时总电导率为7.94×10-3S/cm；初步探讨了Ce_(0.8)Sm_(0.2-x)Y_xO_(1.9)电解质材料的导电机理；
(2)采用化学共沉淀法制备出了5x (x=0,0.2,0.4)粉体材料,经传统烧结制度获得了陶瓷烧结块体材料；以XRD和交流阻抗等分析测试手段对电解质材料的微观结构和性能进行了表征；对La~(3+)的含量对其导电性能的影响进行了研究。结果表明,过量La~(3+)的加入能够很大程度的提高电解质材料的离子电导率,从x=0到x=0.4,电导率从2.5×10-4 S·cm~(-1)提高至1.48×10-3S·cm~(-1),提高了约6倍；利用Jonscher经验公式对其导电过程机理进行了初步探讨,认为长程导电机制在该种电解质材料的导电过程中占主导地位。
(3)采用复合技术制备出了复合氧离子导电体；分别利用共沉淀法、溶剂热法和球磨等方法引入第二相制备出了具有不同复合量的Ce_(0.8)Sm_(0.2)0_(1.9)-La_(9.33)Si_6O_(26)复合电解质材料；采用传统的烧结工艺过程获得了相应的烧结块体复合电解质陶瓷材料；利用XRD、SEM、EDS和交流阻抗技术等检测手段对其物相组成和导电性能进行了表征。研究发现经复合后形成了由Ce0.8Sm0.2O1.9和La_(9.33)Si_6O_(26)两种物相所组成的复合材料体系；认为在复合电解质的导电过程中,两相间的界面效应对于总电导率的提高有着重要的作用；探讨了第二相的复合量和引入手段对于复合电解质导电性能的影响。
(4)利用两步共沉淀法合成了Ce0.8Sm0.1Y0.1O1.9-La9.73Si6O26.6复合电解质材料,利用交流阻抗分析技术对其导电性能进行了测试,结果表明,复合相的相纯度以及界面处固溶反应的发生对于复合电解质的导电性能具有重要影响。
Solid oxide fuel cell (SOFC) is an all-solid-state energy device which could convert directly the chemical energy of fuels and oxidants into electrical energy. At present the most electrolyte materials used in the SOFC system are yttrium stable zirconia (YSZ). YSZ requires a high operating temperature (900-1000℃) to get high enough ionic conductivity, and this will cause problems such as the chemical reaction of battery components, electrode sintering and thermal expansion coefficient mismatch. Ce0.8Sm0.2O1.9-based electrolytes with a fluorite structure and La_(9.33)Si_6O_(26)-based electrolytes with an apatite structure were studied in this thesis. Influences of doping and composite technology on the conductive properties of these two electrolyte materials were studied. The research work comprises the following aspects.
(1) Chemical co-precipitation method was employed to synthesize the Ce_(0.8)Sm_(0.2-x)Y_xO_(1.9)(x=0,0.05,0.1,0.15) powers and the conventional sintering technique was utilized to prepare the related ceramics. The structure and electrical properties of the electrolyte materials were characterized by XRD, SEM and ac impedance technology, respectively. The influence of Y~(3+) contents on the electrical properties of Ce_(0.8)Sm_(0.2-x)Y_xO_(1.9) ceramics was studied. With Y~(3+) content increases, electrical conductivities of electrolytes increase first and then decrease and reach a maximum value when x=0.1, the total conductivity is 7.94×10-3 S·cm~(-1) at 700℃. The conductive mechanism was discussed preliminary.
(2) Chemical co-precipitation method was employed to synthesize the La9.3~(3+)xSi6O26+1.5x (x=0,0.2,0.4) powers and the conventional sintering technique was utilized to prepare the related ceramics. The structure and electrical properties of the electrolyte materials were characterized by XRD and ac impedance technology. The influence of La~(3+) contents on the electrical properties of La9.3~(3+)xSi6O26+1.5x ceramics was studied. Addition of excessive La~(3+) could enhance obviously electrical conductivities of electrolytes. From x=0 to x=0.4, conductivities increase from 2.5×10-4Scm~(-1)to 1.48×10-3S·cm~(-1) at 700℃, about 6 times improved. The conductive mechanism was discussed with Jonscher experience formula, and long-range conduction mechanism was regarded as the dominant one.
(3) Ce0.8Sm0.201.9-La9.33Si6026.6 composite oxygen ion conductors were prepared by composite technology. The second phase was introduced via chemical co-precipitation, solvothermal and ball milling mixing. The composite electrolyte materials with different composite amounts were prepared. The conventional sintering technique was utilized to prepare the related ceramics. The phase and electrical properties of the electrolyte materials were characterized by XRD, SEM, EDS and ac impedance technology. The results show that composite electrolytes consist of Ce0.8Sm0.2O19 and La9.33Si6026-Interfaces between phases play important role in total conductivities. The influences of quantity and introducing way of the second phase on the composites conductive properties were studied.
(4) Ce0.8Sm0.1Y0.1O1.9-La9.73Si6026 composite electrolyte was prepared by two-step co-precipitation method. The electrical properties were characterized by ac impedance technology. The results showed that phase purity and solid solution reaction between interfaces have important influences on the performances of composite electrolytes.
引文
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