中空纤维固体氧化物燃料电池的研究
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摘要
固体氧化物燃料电池（Solid oxide fuel cell，SOFC）是一种可以将化学燃料中的化学能直接、环保和高效地转化成电能的装置。外径在毫米级别的微管式固体氧化物燃料电池具有低的运行温度，优异的抗热循环性能，快速启动能力和更高的体积功率密度。到目前为止，制备微管式固体氧化物燃料电池的主要方法有等静压法、挤出成型法和离心浇铸法等。相转化/纺丝最近被用于制备中空纤维固体氧化物燃料电池（Hollow fibersolid oxide fuel cell，HF-SOFC），它可以更快地制备并且可以更好地控制微观结构。本论文利用相转化/纺丝/共烧结工艺和浸涂、刷涂等方法制备出直型电解质支撑HF-SOFCNiO-YSZ/YSZ/YSZ-LSM/LSM，直型阳极支撑HF-SOFC NiO-YSZ/YSZ/PLNCG，直型阳极支撑HF-SOFC NiO-GDC/GDC/PLNCG，U型阳极支撑HF-SOFC NiO-YSZ/YSZ/YSZ-LSM/LSM和直型阳极支撑HF-SOFC NiO-YSZ/YSZ/YSZ-LSM/LSM。将制备好的各HF-SOFC单电池安装好之后，进行电化学性能测试。本论文主要开展的研究内容如下：
第一，用相转化/纺丝/共烧结技术成功制备出具有非对称结构的直型YSZ电解质中空纤维支撑体，其内侧为指状孔结构，为NiO-YSZ阳极的沉积提供场所，扩大阳极三相区；外侧为非常薄的海绵状孔结构，于一定温度煅烧之后形成很薄的致密层，既可以阻隔阳极氢气和阴极氧气的互相扩散，又可以降低电解质的氧离子传导阻力。在已制备的直型YSZ电解质中空纤维支撑体的基础上，成功制备出直型YSZ电解质支撑HF-SOFC NiO-YSZ/YSZ/YSZ-LSM/LSM，该电池在800oC时的最大功率密度是0.2mWcm-2。
第二，用相转化/纺丝/共烧结技术成功制备出具有非对称结构的直型NiO-YSZ中空纤维阳极支撑体，其内侧为指状孔结构，外侧为海绵状孔结构。在已制备的直型中空纤维NiO-YSZ阳极支撑体的基础上，成功制备出直型阳极支撑HF-SOFC NiO-YSZ/YSZ/PLNCG。该电池表现出良好的电化学性能，其在750oC下电池最大功率密度为876mWcm-2，极化电阻为0.41Ω cm~2且电池在中温区域运行时，PLNCG阴极表现出良好的抗二氧化碳性能。
第三，用相转化/纺丝/共烧结技术成功制备出具有非对称结构的直型NiO-GDC中空纤维阳极支撑体，其内侧为指状孔结构，外侧为海绵状孔结构。XRD图谱表明，PLNCG阴极与GDC电解质在温度不高于900oC的条件下，具有良好的化学兼容性。在已制备的直型中空纤维NiO-GDC阳极支撑体的基础上，成功制备出直型阳极支撑HF-SOFCNiO-GDC/GDC/PLNCG。该电池表现出良好的电化学性能，其在550oC下的最大功率密度为109mW cm-2和极化电阻为0.98Ω cm~2。
第四，用相转化/纺丝/共烧结技术成功制备出U型NiO-YSZ中空纤维阳极支撑体，其内侧为指状孔结构，为阳极燃料气体氢气的输入和产物水蒸气的输出提供良好的传输通道；外侧为海绵状孔结构，其作为阳极三相区，为电池阳极的氢催化氧化反应提供良好的反应场所；在此支撑体的基础上，成功制备出U型阳极支撑HF-SOFCNiO-YSZ/YSZ/YSZ-LSM/LSM。由于YSZ-LSM复合阴极层的使用和LSM阴极集流层的存在，使得电池表现出良好的电化学性能，其在750oC下电池最大功率密度为884mWcm-2，极化电阻为0.36Ω cm~2。该电池表现出良好的热循环性能和稳定性，共经历了65个热循环，并在65个热循环之后又经过了100h的稳定运行，电池稳定运行的总时间达到425h。
Solid oxide fuel cell (SOFC) is a kind of device that convert the chemical energy in thechemical fuels into electrical energy directly, environmentally friendly and efficiently. Themicro tubular solid oxide fuel cell with outer diameter at the millimeter scale possesses lowoperation temperature, excellent performance of resistance of thermal cycling, rapid start-upability and higher volume power density. Up to now, the most common techniques forpreparation micro tubular SOFCs are cold isostatic pressing, extrusion and casting. Phaseinversion/spinning has been recently employed for the fabrication of hollow fber SOFCs(HF-SOFCs), which provides a rapid fabrication process and better control of themicrostructure. In this dissertation, we adopt the phase inversion/spinning/co-sinteringprocess and the dip-coating and brush painting method to prepare the linearelectrolyte-supported HF-SOFC NiO-YSZ/YSZ/YSZ-LSM/LSM, linear anode-supportedHF-SOFC NiO-YSZ/YSZ/PLNCG, linear anode-supported HF-SOFC NiO-GDC/GDC/PLNCG, U-shaped anode-supported HF-SOFC NiO-YSZ/YSZ/YSZ-LSM/LSM and linearanode-supported HF-SOFC NiO-YSZ/YSZ/YSZ-LSM/LSM。After fixing all kinds of theHF-SOFC single cells, we conduct the test of their electrochemical performance. The mainresearch contents of this dissertation are displayed as follows:
Firstly, we successfully fabricate the linear YSZ electrolyte hollow fiber support withasymmetric structure by phase inversion/spinning/co-sintering method. The inner side of theYSZ electrolyte hollow fiber is the finger-like structure, proving the deposition location of theNiO-YSZ anode and enlarging the anode triple phase boundries. The outer side of the YSZelectrolyte hollow fiber is the sponge-like structure, after sintering at certain temperature, itcan form a very thin layer, which both prevent the mutual diffusion of the H2at anode and theO2at cathode and reduce the resistance of the conductivity of O2-. Based on the YSZelectrolyte support, we successfully fabricated the linear electrolyte-supported HF-SOFCNiO-YSZ/YSZ/YSZ-LSM/LSM. The maximum power density of the cell is0.2mW cm-2at750oC.
Secondly, we successfully fabricate the linear NiO-YSZ anode hollow fiber support withasymmetric structure by phase inversion/spinning/co-sintering method, the inner side ofwhich is the finger-like structure and the outer side of which is the sponge-like structure.Based on the NiO-YSZ anode support, we successfully fabricate the linear anode-supportedHF-SOFC NiO-YSZ/YSZ/PLNCG. The cell manifests good electrochemical performance, themaximum power density is876mW cm-2and the polarization resistance is0.41Ω cm~2at750 oC. Moreover, the PLNCG cathode shows good CO2resistance in the intermediatetemperature range.
Thirdly, we successfully fabricate the linear NiO-GDC anode hollow fiber support withasymmetric structure by phase inversion/spinning/co-sintering method, the inner side ofwhich is the finger-like structure and the outer side of which is the sponge-like structure. TheXRD patterns reveal that the PLNCG cathode shows good chemical compatibility with theGDC electrolyte when the temperature is not higher than900oC. Based on the NiO-GDCanode support, we successfully fabricate the linear anode-supported HF-SOFCNiO-GDC/GDC/PLNCG. The cell manifests good electrochemical performance, themaximum power density is109mW cm-2and the polarization resistance is0.98Ω cm~2at550oC.
Fourthly, we successfully fabricate the U-shaped NiO-YSZ anode hollow fiber supportby phase inversion/spinning/co-sintering method, the inner side of which is the finger-likestructure, providing the deliver channels for the importing of the H2fuel gas and exporting ofthe product vapor; the outer side of which is the sponge-like structure, containing the anodetriple phase boundries, providing the reaction sites for the catalytic oxidation of the H2in theanode. Based on the support, we successfully fabricated the U-shaped anode-supportedHF-SOFC NiO-YSZ/YSZ/YSZ-LSM/LSM. By using of the YSZ-LSM composite cathodelayer and existing of the LSM cathode current collection layer, the cell manifests goodelectrochemical performance, the maximum power density is884mW cm-2and thepolarization resistance is0.36Ω cm~2at750oC. Moreover, the cell shows good thermalcycling performance and stability, undergoing65thermal cycles; after the65thermal cycles,the cell works for additional100h. The total stabilized operation time of the cell is425h.
第一，用相转化/纺丝/共烧结技术成功制备出具有非对称结构的直型YSZ电解质中空纤维支撑体，其内侧为指状孔结构，为NiO-YSZ阳极的沉积提供场所，扩大阳极三相区；外侧为非常薄的海绵状孔结构，于一定温度煅烧之后形成很薄的致密层，既可以阻隔阳极氢气和阴极氧气的互相扩散，又可以降低电解质的氧离子传导阻力。在已制备的直型YSZ电解质中空纤维支撑体的基础上，成功制备出直型YSZ电解质支撑HF-SOFC NiO-YSZ/YSZ/YSZ-LSM/LSM，该电池在800oC时的最大功率密度是0.2mWcm-2。
第二，用相转化/纺丝/共烧结技术成功制备出具有非对称结构的直型NiO-YSZ中空纤维阳极支撑体，其内侧为指状孔结构，外侧为海绵状孔结构。在已制备的直型中空纤维NiO-YSZ阳极支撑体的基础上，成功制备出直型阳极支撑HF-SOFC NiO-YSZ/YSZ/PLNCG。该电池表现出良好的电化学性能，其在750oC下电池最大功率密度为876mWcm-2，极化电阻为0.41Ω cm~2且电池在中温区域运行时，PLNCG阴极表现出良好的抗二氧化碳性能。
第三，用相转化/纺丝/共烧结技术成功制备出具有非对称结构的直型NiO-GDC中空纤维阳极支撑体，其内侧为指状孔结构，外侧为海绵状孔结构。XRD图谱表明，PLNCG阴极与GDC电解质在温度不高于900oC的条件下，具有良好的化学兼容性。在已制备的直型中空纤维NiO-GDC阳极支撑体的基础上，成功制备出直型阳极支撑HF-SOFCNiO-GDC/GDC/PLNCG。该电池表现出良好的电化学性能，其在550oC下的最大功率密度为109mW cm-2和极化电阻为0.98Ω cm~2。
第四，用相转化/纺丝/共烧结技术成功制备出U型NiO-YSZ中空纤维阳极支撑体，其内侧为指状孔结构，为阳极燃料气体氢气的输入和产物水蒸气的输出提供良好的传输通道；外侧为海绵状孔结构，其作为阳极三相区，为电池阳极的氢催化氧化反应提供良好的反应场所；在此支撑体的基础上，成功制备出U型阳极支撑HF-SOFCNiO-YSZ/YSZ/YSZ-LSM/LSM。由于YSZ-LSM复合阴极层的使用和LSM阴极集流层的存在，使得电池表现出良好的电化学性能，其在750oC下电池最大功率密度为884mWcm-2，极化电阻为0.36Ω cm~2。该电池表现出良好的热循环性能和稳定性，共经历了65个热循环，并在65个热循环之后又经过了100h的稳定运行，电池稳定运行的总时间达到425h。
Solid oxide fuel cell (SOFC) is a kind of device that convert the chemical energy in thechemical fuels into electrical energy directly, environmentally friendly and efficiently. Themicro tubular solid oxide fuel cell with outer diameter at the millimeter scale possesses lowoperation temperature, excellent performance of resistance of thermal cycling, rapid start-upability and higher volume power density. Up to now, the most common techniques forpreparation micro tubular SOFCs are cold isostatic pressing, extrusion and casting. Phaseinversion/spinning has been recently employed for the fabrication of hollow fber SOFCs(HF-SOFCs), which provides a rapid fabrication process and better control of themicrostructure. In this dissertation, we adopt the phase inversion/spinning/co-sinteringprocess and the dip-coating and brush painting method to prepare the linearelectrolyte-supported HF-SOFC NiO-YSZ/YSZ/YSZ-LSM/LSM, linear anode-supportedHF-SOFC NiO-YSZ/YSZ/PLNCG, linear anode-supported HF-SOFC NiO-GDC/GDC/PLNCG, U-shaped anode-supported HF-SOFC NiO-YSZ/YSZ/YSZ-LSM/LSM and linearanode-supported HF-SOFC NiO-YSZ/YSZ/YSZ-LSM/LSM。After fixing all kinds of theHF-SOFC single cells, we conduct the test of their electrochemical performance. The mainresearch contents of this dissertation are displayed as follows:
Firstly, we successfully fabricate the linear YSZ electrolyte hollow fiber support withasymmetric structure by phase inversion/spinning/co-sintering method. The inner side of theYSZ electrolyte hollow fiber is the finger-like structure, proving the deposition location of theNiO-YSZ anode and enlarging the anode triple phase boundries. The outer side of the YSZelectrolyte hollow fiber is the sponge-like structure, after sintering at certain temperature, itcan form a very thin layer, which both prevent the mutual diffusion of the H2at anode and theO2at cathode and reduce the resistance of the conductivity of O2-. Based on the YSZelectrolyte support, we successfully fabricated the linear electrolyte-supported HF-SOFCNiO-YSZ/YSZ/YSZ-LSM/LSM. The maximum power density of the cell is0.2mW cm-2at750oC.
Secondly, we successfully fabricate the linear NiO-YSZ anode hollow fiber support withasymmetric structure by phase inversion/spinning/co-sintering method, the inner side ofwhich is the finger-like structure and the outer side of which is the sponge-like structure.Based on the NiO-YSZ anode support, we successfully fabricate the linear anode-supportedHF-SOFC NiO-YSZ/YSZ/PLNCG. The cell manifests good electrochemical performance, themaximum power density is876mW cm-2and the polarization resistance is0.41Ω cm~2at750 oC. Moreover, the PLNCG cathode shows good CO2resistance in the intermediatetemperature range.
Thirdly, we successfully fabricate the linear NiO-GDC anode hollow fiber support withasymmetric structure by phase inversion/spinning/co-sintering method, the inner side ofwhich is the finger-like structure and the outer side of which is the sponge-like structure. TheXRD patterns reveal that the PLNCG cathode shows good chemical compatibility with theGDC electrolyte when the temperature is not higher than900oC. Based on the NiO-GDCanode support, we successfully fabricate the linear anode-supported HF-SOFCNiO-GDC/GDC/PLNCG. The cell manifests good electrochemical performance, themaximum power density is109mW cm-2and the polarization resistance is0.98Ω cm~2at550oC.
Fourthly, we successfully fabricate the U-shaped NiO-YSZ anode hollow fiber supportby phase inversion/spinning/co-sintering method, the inner side of which is the finger-likestructure, providing the deliver channels for the importing of the H2fuel gas and exporting ofthe product vapor; the outer side of which is the sponge-like structure, containing the anodetriple phase boundries, providing the reaction sites for the catalytic oxidation of the H2in theanode. Based on the support, we successfully fabricated the U-shaped anode-supportedHF-SOFC NiO-YSZ/YSZ/YSZ-LSM/LSM. By using of the YSZ-LSM composite cathodelayer and existing of the LSM cathode current collection layer, the cell manifests goodelectrochemical performance, the maximum power density is884mW cm-2and thepolarization resistance is0.36Ω cm~2at750oC. Moreover, the cell shows good thermalcycling performance and stability, undergoing65thermal cycles; after the65thermal cycles,the cell works for additional100h. The total stabilized operation time of the cell is425h.
引文
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