固体氧化物燃料电池的相转化及流延法制备研究
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摘要
固体氧化物燃料电池(SOFC)是一种可直接将化学能转换为电能的装置,因其具备全固态、高效、环境友好等众多优点而受到人们的日益关注。传统的高温SOFC对电池材料和制备技术的要求较高,导致了电池的制备成本过高,限制了SOFC的实际应用。因此降低SOFC的工作温度已成为目前SOFC主要的研究方向。
制备薄膜电解质是实现SOFC的中低温操作的最有效方式之一,为了实现中低温SOFC的低成本和实用化目标,本论文主要侧重于阳极支撑的SOFC的制备工艺技术研究以及电化学性能表征上。此外,为了避开含钴阴极的不利影响,论文也对新型无钻钙钛矿阴极材料La0.6Ba0.4Fe1-xNixO3-δ的性能进行了研究。
论文第一章概述了SOFC的工作原理、关键材料、发展趋势以及制备方法等。针对SOFC市场化面临的制备技术和阴极材料的挑战,提出了本论文的研究目标及研究内容。
第二章中发展了相转化与真空辅助浸渍相结合的方法制备了阳极支撑的管状SOFC。首先用相转化法制备了NiO-YSZ(氧化钇稳定的氧化锆)阳极支撑体,再利用真空辅助浸渍技术来制备YSZ电解质薄膜。经过1400℃共烧后,成功的在1000℃预烧的NiO-YSZ阳极衬底上制备出了非常致密的YSZ电解质薄膜。以La0.8Sr0.2MnO3-δ-YSZ (LSM-YSZ)为复合阴极,单电池在700℃获得的最大功率密度为155mW/cm2。此外,通过引入阳极功能层使电池的性能进一步得到提高。研究表明相转化结合真空辅助浸渍技术是制备阳极支撑的管状SOFC的一种简便有效的方法。
第三章作者研究了相转化方法制备了基于Ce0.8Sm0.2O2-δ(SDC)的中空纤维陶瓷管SOFC。纤维管NiO-SDC阳极衬底采用相转化法制备,在阳极衬底上采用真空辅助浸渍成功制备了20μm厚的SDC电解质。采用潮湿的氢气为燃料气,单电池在600℃获得的最大功率密度和开路电压分别为168mW/cm2和0.71V。此外,通过制备一层电子阻隔层显著地提高了此电池的开路电压。由于纤维管SOFC具有非常高的堆积密度,未来应用潜力很大。
第四章我们通过原位相转化法和浆料浸渍的方法成功制备了NiO-BaZr0.1Ce0.7Y0.2O3-δ(NiO-BZCY)阳极支撑体以及厚度约为25μm的BaZr0.8Y0.2O3-δ (BZY)致密电解质薄膜。通过在凝固浴中引入酒精获得了满足需要的阳极衬底。电池表征给出,在550℃、600℃和650℃的功率密度分别是34、55和70mW/cm2,比传统的电解质支撑的BZY电池高出近一个数量级。实验表明相转化法制备平板状SOFC是非常可行的。
第五章提出了通过流延、喷雾工艺制备阳极支撑的质子导体SOFC。 NiO-BZCY阳极衬底是利用流延法制备并对预烧温度优化后得到的。致密的BaZr0.1Ce0.7Y0.2O3-δ(BZCY)电解质是通过简单的喷雾技术制备的。电池在550℃获得了97mW/cm2的功率输出。另外,我们还将流延法应用于阳极支撑的单电池NiO-BZCY/BZY/Sm0.5Sr0.5CoO3-δ-SDC的制备中,获得的单电池在600℃的最大功率密度为91mW/cm2,其数值与当前的BZY薄膜电池性能的发展水平相当。实验结果充分证明流延结合喷雾技术是低成本制备阳极支撑的质子陶瓷膜燃料电池的可靠性路径。
第六章对钙钛矿氧化物La0.6Ba0.4Fe1-xNixO3-δ (LBFN)作为中低温SOFC的一种无钴阴极的潜能进行了探索研究。电导率测试表明,电导率随着Ni掺杂量的增加而增加,La0.6Ba0.4Fe0.8Ni0.2O3-δ (LBFN2)在450℃的电导率达到了300S/cm。XRD表明,LBFN2与SDC的兼容性非常好。LBFN2-SDC/SDC/LBFN2-SDC对称电池的交流阻抗测试表明,LBFN2-SDC(质量比7：3)复合阴极的面极化电阻在700℃只有0.17Ωcm2。以其作为阴极,NiO-SDC阳极支撑20μm厚的SDC薄膜电解质单电池在600℃的最大功率密度达到了300mW/cm2,结果表明LBFN2是有潜力的一种无钴中低温SOFC阴极材料。
论文第七章对本论文的工作进行了总结,并对阳极支撑的SOFC低成本制备技术的后续工作进行了展望。
Solid Oxide Fuel Cell (SOFC) is attracting more and more attention as a direct chemical-to-electrical energy conversion device for its solid-state structure, high efficiency, environmental friendly, etc. Conventional high-temperature SOFC has a strict demand on the materials and fabrication techniques, leading to a high cost on manufacture which limits the practical application of SOFC. Therfore, reducing the SOFC operating temperature is the current research trend.
Fabrication of thin electrolyte membrane is one of the most effective techniques to lower the operating temperature of SOFC. In order to develop intermediate-to-low SOFC with lower cost and achieve practicality, this thesis mainly focuses on fabrication techniques for anode supported SOFC and characterization of the electrochemical performances. Moreover, to avoid the drawbacks of cobalt-based cathodes, novel La0.6Ba0.4Fe1-xNixO3-δ cobalt-free perovskite cathodes are also investigated in this thesis.
Chapter1reviews the operating principle, critical materials, development tendency and preparation of SOFC. Furthermore, we propose that the thesis aims at the challenge of the cathode materials and fabrication techniques in successful industrialization of SOFC.
Chapter2describes the phase inversion method combined with vacuum-assisted coating technique to fabricate the anode-supported tubular SOFC. Phase inversion method was applied to prepare the NiO-YSZ (Yttria-stabilized zirconia) anode support and vacuum assisted coating technique was used to fabricate the YSZ electrolyte membrane. After co-sintered at1400℃, a dense YSZ electrolyte membrane was successfully coated on NiO-YSZ anode substrate pre-sintered at1000℃. With La0.8Sr0.2MnO3-δ-YSZ (LSM-YSZ) as the composite cathode, a maximum power density of155mW/cm2was obtained at700℃for the single cell. Furthermore, the performance was improved significantly by introducing an anode functional layer. Based on the results, the phase inversion method combined with vacuum-assisted coating technique is a simple and efficient process to prepare the anode supported tubular SOFC.
In Chapter3, we prepared and studied anode-supported hollow fiber Ce0.8Sm0.2O2-δ(SDC)-based SOFC. The NiO-Ce0.8Sm0.2O2-δ (NiO-SDC) anode hollow fiber was prepared by the phase inversion method and a20-μm-thick SDC electrolyte membrane was deposited on the anode substrate using vacuum-assisted coating technique. With the wet hydrogen (3%H2O) as the fuel, the single cell exhibited the maximum power density of168mW/cm2and the open-circuit voltage (OCV) of0.71V at600℃. Moreover, the OCV was significantly improved by incorporating an electron-blocking layer. Given the high stacking density of the hollow fiber, the hollow fiber SOFC has a high potential for practical applications.
In chapter4, planar NiO-BaZr0.1Ce0.7Y0.2O3-δ (NiO-BZCY) anode substrates were prepared by the phase inversion method based on in-situ reaction and the thin BaZr0.8Y0.2O3-δ (BZY) electrolyte membranes with the thickness of25μm were fabricated by a dip-coating method. In order to fabricate suitable substrates, ethanol was introduced into the coagulation bath. The single cell generated maximum power densities of34,55and70mW/cm2at550,600and650℃, respectively, the performance of which is almost an order of magnitude higher than that of the electrolyte-supported SOFC based on BZY electrolyte. It can be concluded that the phase inversion process is also a facile method for fabricating planar SOFC.
Chapter5describes a method of tape casting combined with spray coating for preparing the anode-supported proton-conducting SOFC. The NiO-BZCY anode substrates were prepared by tape casting and then pre-sintered at different temperatures. The dense BZCY electrolyte membranes were successfully prepared by a simple suspension spray coating technique. The maximum power density of the single cell achieved97mW/cm2at550℃. In addition, the performance of the single cell (NiO-BaZr0.1Ce0.7Y0.2O3-δ/BaZr0.8Y0.2O3-δ/Sm0.5Sr0.5CoO3-δ-SDC) prepared by spray-tape casting method was also studied. A maximum power density of91mW/cm2was obtained at600℃, which is comparable with the best performance of BZY-based SOFC by far. The results demonstrate the method of tape casting combined with spay coating technique is a low-cost and reliable route to prepare anode-supported proton-conducting SOFC.
In Chapter6, perovskite oxides La0.6Ba0.4Fe1-xNixO3-δ (LBFN) were investigated for potential application as Co-free cathodes for intermediate-to-low SOFC. The conductivities increased with increasing Ni content, and the conductivity of La0.6Ba0.4Fe0.8Ni0.2O3-δ (LBFN2) reached300S/cm at450℃. The XRD results revealed that LBFN2and SDC showed excellent compatibility between each other. The AC impedance spectra of the symmetrical cell LBFN2-SDC/SDC/LBFN2-SDC were also investigated and the area specific resistance (ASR) of LBFN2-SDC (7:3in weight ratio) composite cathode was as low as0.17Qcm2at700℃. Using the LBFN2-SDC (7:3in weight ratio) as the composite cathode, the Ni-SDC support single cell with a20-μm-thick SDC membrane exhibited a desirable maximum power density of300mW/cm2at600℃. The results show that LBFN2might be a potential Co-free cathode material for intermediate-to-low SOFC.
In chapter7, the researches presented in this dissertation are evaluated and future work concerning the cost-effective preparation techniques of anode supported SOFC is discussed.
制备薄膜电解质是实现SOFC的中低温操作的最有效方式之一,为了实现中低温SOFC的低成本和实用化目标,本论文主要侧重于阳极支撑的SOFC的制备工艺技术研究以及电化学性能表征上。此外,为了避开含钴阴极的不利影响,论文也对新型无钻钙钛矿阴极材料La0.6Ba0.4Fe1-xNixO3-δ的性能进行了研究。
论文第一章概述了SOFC的工作原理、关键材料、发展趋势以及制备方法等。针对SOFC市场化面临的制备技术和阴极材料的挑战,提出了本论文的研究目标及研究内容。
第二章中发展了相转化与真空辅助浸渍相结合的方法制备了阳极支撑的管状SOFC。首先用相转化法制备了NiO-YSZ(氧化钇稳定的氧化锆)阳极支撑体,再利用真空辅助浸渍技术来制备YSZ电解质薄膜。经过1400℃共烧后,成功的在1000℃预烧的NiO-YSZ阳极衬底上制备出了非常致密的YSZ电解质薄膜。以La0.8Sr0.2MnO3-δ-YSZ (LSM-YSZ)为复合阴极,单电池在700℃获得的最大功率密度为155mW/cm2。此外,通过引入阳极功能层使电池的性能进一步得到提高。研究表明相转化结合真空辅助浸渍技术是制备阳极支撑的管状SOFC的一种简便有效的方法。
第三章作者研究了相转化方法制备了基于Ce0.8Sm0.2O2-δ(SDC)的中空纤维陶瓷管SOFC。纤维管NiO-SDC阳极衬底采用相转化法制备,在阳极衬底上采用真空辅助浸渍成功制备了20μm厚的SDC电解质。采用潮湿的氢气为燃料气,单电池在600℃获得的最大功率密度和开路电压分别为168mW/cm2和0.71V。此外,通过制备一层电子阻隔层显著地提高了此电池的开路电压。由于纤维管SOFC具有非常高的堆积密度,未来应用潜力很大。
第四章我们通过原位相转化法和浆料浸渍的方法成功制备了NiO-BaZr0.1Ce0.7Y0.2O3-δ(NiO-BZCY)阳极支撑体以及厚度约为25μm的BaZr0.8Y0.2O3-δ (BZY)致密电解质薄膜。通过在凝固浴中引入酒精获得了满足需要的阳极衬底。电池表征给出,在550℃、600℃和650℃的功率密度分别是34、55和70mW/cm2,比传统的电解质支撑的BZY电池高出近一个数量级。实验表明相转化法制备平板状SOFC是非常可行的。
第五章提出了通过流延、喷雾工艺制备阳极支撑的质子导体SOFC。 NiO-BZCY阳极衬底是利用流延法制备并对预烧温度优化后得到的。致密的BaZr0.1Ce0.7Y0.2O3-δ(BZCY)电解质是通过简单的喷雾技术制备的。电池在550℃获得了97mW/cm2的功率输出。另外,我们还将流延法应用于阳极支撑的单电池NiO-BZCY/BZY/Sm0.5Sr0.5CoO3-δ-SDC的制备中,获得的单电池在600℃的最大功率密度为91mW/cm2,其数值与当前的BZY薄膜电池性能的发展水平相当。实验结果充分证明流延结合喷雾技术是低成本制备阳极支撑的质子陶瓷膜燃料电池的可靠性路径。
第六章对钙钛矿氧化物La0.6Ba0.4Fe1-xNixO3-δ (LBFN)作为中低温SOFC的一种无钴阴极的潜能进行了探索研究。电导率测试表明,电导率随着Ni掺杂量的增加而增加,La0.6Ba0.4Fe0.8Ni0.2O3-δ (LBFN2)在450℃的电导率达到了300S/cm。XRD表明,LBFN2与SDC的兼容性非常好。LBFN2-SDC/SDC/LBFN2-SDC对称电池的交流阻抗测试表明,LBFN2-SDC(质量比7：3)复合阴极的面极化电阻在700℃只有0.17Ωcm2。以其作为阴极,NiO-SDC阳极支撑20μm厚的SDC薄膜电解质单电池在600℃的最大功率密度达到了300mW/cm2,结果表明LBFN2是有潜力的一种无钴中低温SOFC阴极材料。
论文第七章对本论文的工作进行了总结,并对阳极支撑的SOFC低成本制备技术的后续工作进行了展望。
Solid Oxide Fuel Cell (SOFC) is attracting more and more attention as a direct chemical-to-electrical energy conversion device for its solid-state structure, high efficiency, environmental friendly, etc. Conventional high-temperature SOFC has a strict demand on the materials and fabrication techniques, leading to a high cost on manufacture which limits the practical application of SOFC. Therfore, reducing the SOFC operating temperature is the current research trend.
Fabrication of thin electrolyte membrane is one of the most effective techniques to lower the operating temperature of SOFC. In order to develop intermediate-to-low SOFC with lower cost and achieve practicality, this thesis mainly focuses on fabrication techniques for anode supported SOFC and characterization of the electrochemical performances. Moreover, to avoid the drawbacks of cobalt-based cathodes, novel La0.6Ba0.4Fe1-xNixO3-δ cobalt-free perovskite cathodes are also investigated in this thesis.
Chapter1reviews the operating principle, critical materials, development tendency and preparation of SOFC. Furthermore, we propose that the thesis aims at the challenge of the cathode materials and fabrication techniques in successful industrialization of SOFC.
Chapter2describes the phase inversion method combined with vacuum-assisted coating technique to fabricate the anode-supported tubular SOFC. Phase inversion method was applied to prepare the NiO-YSZ (Yttria-stabilized zirconia) anode support and vacuum assisted coating technique was used to fabricate the YSZ electrolyte membrane. After co-sintered at1400℃, a dense YSZ electrolyte membrane was successfully coated on NiO-YSZ anode substrate pre-sintered at1000℃. With La0.8Sr0.2MnO3-δ-YSZ (LSM-YSZ) as the composite cathode, a maximum power density of155mW/cm2was obtained at700℃for the single cell. Furthermore, the performance was improved significantly by introducing an anode functional layer. Based on the results, the phase inversion method combined with vacuum-assisted coating technique is a simple and efficient process to prepare the anode supported tubular SOFC.
In Chapter3, we prepared and studied anode-supported hollow fiber Ce0.8Sm0.2O2-δ(SDC)-based SOFC. The NiO-Ce0.8Sm0.2O2-δ (NiO-SDC) anode hollow fiber was prepared by the phase inversion method and a20-μm-thick SDC electrolyte membrane was deposited on the anode substrate using vacuum-assisted coating technique. With the wet hydrogen (3%H2O) as the fuel, the single cell exhibited the maximum power density of168mW/cm2and the open-circuit voltage (OCV) of0.71V at600℃. Moreover, the OCV was significantly improved by incorporating an electron-blocking layer. Given the high stacking density of the hollow fiber, the hollow fiber SOFC has a high potential for practical applications.
In chapter4, planar NiO-BaZr0.1Ce0.7Y0.2O3-δ (NiO-BZCY) anode substrates were prepared by the phase inversion method based on in-situ reaction and the thin BaZr0.8Y0.2O3-δ (BZY) electrolyte membranes with the thickness of25μm were fabricated by a dip-coating method. In order to fabricate suitable substrates, ethanol was introduced into the coagulation bath. The single cell generated maximum power densities of34,55and70mW/cm2at550,600and650℃, respectively, the performance of which is almost an order of magnitude higher than that of the electrolyte-supported SOFC based on BZY electrolyte. It can be concluded that the phase inversion process is also a facile method for fabricating planar SOFC.
Chapter5describes a method of tape casting combined with spray coating for preparing the anode-supported proton-conducting SOFC. The NiO-BZCY anode substrates were prepared by tape casting and then pre-sintered at different temperatures. The dense BZCY electrolyte membranes were successfully prepared by a simple suspension spray coating technique. The maximum power density of the single cell achieved97mW/cm2at550℃. In addition, the performance of the single cell (NiO-BaZr0.1Ce0.7Y0.2O3-δ/BaZr0.8Y0.2O3-δ/Sm0.5Sr0.5CoO3-δ-SDC) prepared by spray-tape casting method was also studied. A maximum power density of91mW/cm2was obtained at600℃, which is comparable with the best performance of BZY-based SOFC by far. The results demonstrate the method of tape casting combined with spay coating technique is a low-cost and reliable route to prepare anode-supported proton-conducting SOFC.
In Chapter6, perovskite oxides La0.6Ba0.4Fe1-xNixO3-δ (LBFN) were investigated for potential application as Co-free cathodes for intermediate-to-low SOFC. The conductivities increased with increasing Ni content, and the conductivity of La0.6Ba0.4Fe0.8Ni0.2O3-δ (LBFN2) reached300S/cm at450℃. The XRD results revealed that LBFN2and SDC showed excellent compatibility between each other. The AC impedance spectra of the symmetrical cell LBFN2-SDC/SDC/LBFN2-SDC were also investigated and the area specific resistance (ASR) of LBFN2-SDC (7:3in weight ratio) composite cathode was as low as0.17Qcm2at700℃. Using the LBFN2-SDC (7:3in weight ratio) as the composite cathode, the Ni-SDC support single cell with a20-μm-thick SDC membrane exhibited a desirable maximum power density of300mW/cm2at600℃. The results show that LBFN2might be a potential Co-free cathode material for intermediate-to-low SOFC.
In chapter7, the researches presented in this dissertation are evaluated and future work concerning the cost-effective preparation techniques of anode supported SOFC is discussed.
引文
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