便携式锥管状固体氧化物燃料电池的研究与开发
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摘要
固体氧化物燃料电池（SOFC）采用固体陶瓷材料作为电解质，是一种高效、环境友好的全固态电化学发电装置，具有广泛的应用前景。锥管串接式SOFC可以使电堆在较小的空间内有相对高的电压和输出，良好的抗热冲击性和热循环能力，特别适合于重量轻、体积小的SOFC电堆便携式能源领域应用。本论文围绕锥管状SOFC的便携式应用这个主题展开，主要对锥管状SOFC的制备工艺、新型电极材料及其抗积碳机理、便携式直接碳固体氧化物燃料电池（DC-SOFC）进行了研究与开发，旨在推进锥管状SOFC的便携式应用的产业化进程。
本论文采用凝胶注模成型法成功制备了锥管状阳极生坯，并组装成单电池和电池组，对其电化学性能进行了研究。研究表明，采用凝胶注模成型法制备的电池微观结构较理想，将阳极生坯和电解质在1350°C共烧结制备的电解质致密，并与阳极和阴极接触良好。制备的单电池在750°C和800°C以氢气为燃料时最大功率密度分别为600mW/cm~2和900mW/cm~2，开路电压约为1V。制备的三节串联电堆以加湿氢气为燃料800°C最大功率输出为2.8W，以加湿甲烷为燃料时电堆在800°C和850°C的最大输出功率分别达到3.0W和4.0W，说明采用凝胶注模成型工艺制备的电池性能较好。电堆在850°C以甲烷为燃料10mA/cm~2的恒电流密度下放电4.5h后电堆的性能下降，因此寻找抗积碳的新型阳极使SOFC在碳氢化合物中稳定运行是非常必要的。
本论文开发了一种新型阳极材料(Ni_(0.75)Fe_(0.25)-5MgO)/YSZ。通过对合成的Ni_(0.75)Fe_(0.25)O粉体进行XRD表征发现， Fe已经进入了NiO的立方晶格，形成了Ni_(0.75)Fe_(0.25)O固溶体。研究了MgO的掺杂量对SOFC性能的影响，结果表明，阳极中加入一定量的Fe和MgO后，电池的最大功率密度增大，但加入过多的MgO其性能反而下降。以(Ni_(0.75)Fe_(0.25)-5MgO)/YSZ为阳极的SOFC使用加湿甲烷为燃料时800°C的最大输出功率达到648mW/cm~2，确定了MgO的最佳掺杂量为5wt.%。不同阳极的SOFC的恒电流放电曲线表明，以Ni0.75Fe0.25/YSZ为阳极的SOFC在甲烷中很快衰减，当阳极中加入一定量的MgO后，电压在整个20h的测试过程中保持相对稳定。原因可能是阳极中加入一定量的稳定金属氧化物MgO可以抑制碳纤维的生长，或者使得YSZ骨架有足够的机械强度来承受由于碳纤维的生长对其产生的应力。对各电池经稳定性测试后阳极SEM图的分析结果进一步证实了上述机理推测。本章充分证明了(Ni0.75Fe0.25–5MgO)/YSZ阳极在直接使用甲烷为燃料的锥管状固体氧化物燃料电池中应用的可行性。
在上述研究工作的基础上，研究了以(Ni_(0.75)Fe_(0.25)-5MgO)/YSZ为阳极的SOFC直接使用CO为燃料的性能。结果表明，以H2为燃料的电池性能都要高于以CO为燃料的性能，而以干燥CO为燃料的电池性能都要高于以加湿CO为燃料的性能。稳定性测试表明，以(Ni_(0.75)Fe_(0.25)-5MgO)/YSZ为阳极的单电池在800°C以83mA/cm~2的恒电流测试的40h内电压都相当稳定，而以Ni/YSZ为阳极的单电池工作了10h后电压快速下降为零，并且水对以(Ni_(0.75)Fe_(0.25)-5MgO)/YSZ为阳极的单电池使用CO为燃料时的稳定性没有影响。SEM测试结果表明，使用CO为燃料时，在Ni/YSZ阳极表面的积碳比(Ni_(0.75)Fe_(0.25)-5MgO)/YSZ阳极的严重。制备的两节串联电堆使用加湿CO为燃料时，在800°C的开路电压和最大输出分别为2V和4W，电堆在以83mA/cm~2的恒电流密度下放电的90h内表现出良好的稳定性，进一步证明(Ni_(0.75)Fe_(0.25)-5MgO)/YSZ新型阳极非常适合于固体氧化物燃料电池使用含碳燃料的便携式应用。
本论文设计并开发了一种适合于直接碳固体氧化物燃料电池便携式应用的装置。证明了碳燃料中加入适量的FemOn能催化炭的Boudouard反应，提高电池性能。以担载5wt.%Fe催化剂的活性炭为燃料，制备的便携式DC-SOFC单电池850°C的开路电压达1.05V，最大功率密度达到280mW/cm~2。寿命测试结果表明，电池以小电流放电时，电压维持较稳定，随着运行电流的增大，电池的寿命减小。小电流放电后容器内剩余的红褐色粉末经EDX测试分析主要为铁的氧化物，表明炭已消耗完。制备的便携式三节串联DC-SOFC电池组使用担载5wt.%Fe的活性炭为燃料时电化学性能较低。这是由于该便携式装置的密封难度大，如何解决该装置的密封问题也是今后我们工作的重点。
Solid oxide fuel cell (SOFC) is a highly efficient, environment friendly and all-solid-state electrochemical power generation device, which uses a solid ceramic material as theelectrolyte and has a wide range of applications. The cone-shaped tubular segmented-in-seriesSOFC design can achieve a relatively higher voltage and power in a limited space, goodthermal shock resistance and thermal cycling capability, so that it is specially suitable forSOFC stack for portable applications, which need light weight and compact volume. Thisthesis centers around the research and development of technique to frabricate cone-shapedtubular SOFC, new anode material and its anti-coking mechanism, a novel direct carbon solidoxide fuel cell (DC-SOFC) device to speed up the industrialization process of cone-shapedtubular SOFC for portable application.
Gel-casting technique is developed to fabricate the green cone-shaped anode substratesand the performance of a single cell and stack are investigated. The results show that themicrostructure of the cell fabricated by gel-casting technique is ideal, YSZ electrolyte filmfabricated by co-sintering of the electrolyte and green anode substrates is dense and adhereswell to both the anode and cathode. The maximum power density of the single cell usinghydrogen as fuel is about600and900mW/cm~2at750°C and800°C, respectively. The opencircuit voltage (OCV) is about1V. The maximum output power of the three-cell-stack usinghydrogen as fuel is about2.8W. When using methane as fuel, the maximum output power is3.0and4.0W at800°C and850°C. It means that the performance of the cell fabricated bygel-casting technique is fine. The performance of the stack decreases when measured under aconstant current density of10mA/cm~2at850°C using humidified methane as fuel. So findingnew anode material with anti-coking ability for SOFC using hydrocarbons as fuel isimperative.
A new anode material (Ni_(0.75)Fe_(0.25)-5MgO)/YSZ is developed. The X-ray spectrum of thefabricated Ni_(0.75)Fe_(0.25)O power indicats that Fe was doped into the crystal structure of NiO,forming a solid Ni1xFexO solution. The results show that the power density increases as aproper amount of Fe and MgO is doped into the anode, while the performance decreases astoo much MgO is added into the anode. A maximum power density of648mW/cm~2at0.7Vand800°C for the SOFC with (Ni_(0.75)Fe_(0.25)-5MgO)/YSZ anode is achieved using humidifiedmethane as fuel. The stability test results for the cells with different anodes show that the cellwith Ni0.75Fe0.25/YSZ anode fails rapidly in methane. When MgO is added into the bulk anode,the voltage remains stable over the whole period of20h. This may be explaned as follows: on the one hand, the doped stable oxide MgO can suppress carbon fiber growth; on the otherhand, MgO particles located on the grain boundaries of YSZ make the YSZ skeleton strongenough to stand the stress caused by carbon fiber growth. SEM micrographs of the anodesubstrates of the single cells after the output performance and stability test further strengthenthe mechanisms above. This proves that (Ni0.75Fe0.25–5MgO)/YSZ is a promising anodematerial for cone-shaped tubular SOFCs operated on methane fuel.
Based on the works above, we have researched on the performance of SOFCs with(Ni_(0.75)Fe_(0.25)-5MgO)/YSZ anode using CO as fuel. For the cell with either of the anodes, theperformance on hydrogen is better than that on CO, and that on moist CO is poorer than ondry CO. The durability results show that while the cells with traditional Ni/YSZ anode failafter operating on either dry or moist CO for about10h, the voltage of the cells with(Ni_(0.75)Fe_(0.25)-5MgO)/YSZ anode remains stable during the whole test time (40h). And thepresence of water in CO fuel has no effect on the stability of cell with (Ni0.75Fe0.25-5%MgO)/YSZ anode. SEM images of the surface of the anodes after output performance andstability test shows that cells with Ni/YSZ anodes have more deposition than (Ni0.75Fe0.25-5MgO)/YSZ anode when using CO as fuel. The OCV of the two-cell-stack with (Ni0.75Fe0.25-5MgO)/YSZ anode is2V and its maximum output power is4W at800°C. A durability testof the two-cell-stack on moist CO is performed at a constant current density of83mAcm2. Itindicates that the stability of the as-prepared two-cell-stack with (Ni_(0.75)Fe_(0.25)-5MgO)/YSZanode is good during the whole testing time of90h. This character is very significant for theportable application of SOFCs operated on carbon fuel.
A portable device has been designed for the application of direct carbon solid oxide fuelcell. The results show that Fe catalyst catalyses the Boudouard reaction of cabon fuel andimproves the cell performance. The OCV of the single DC-SOFC is1.05V and its maximumoutput power density is280mW/cm~2at850°C. Stability test results show that the voltage canremain stable when the operating current is small and larger operating current resulted inshorter operation life. EDX analysis shows that the reddish fuel residue is mainly Fe2O3andindicates carbon fuel is depleted. The performance of the three-cell DC-SOFC stack forportable application is poor. For sealing is difficult for this portable device, further work isnecessary to solve the sealing problems of this portable device.
本论文采用凝胶注模成型法成功制备了锥管状阳极生坯，并组装成单电池和电池组，对其电化学性能进行了研究。研究表明，采用凝胶注模成型法制备的电池微观结构较理想，将阳极生坯和电解质在1350°C共烧结制备的电解质致密，并与阳极和阴极接触良好。制备的单电池在750°C和800°C以氢气为燃料时最大功率密度分别为600mW/cm~2和900mW/cm~2，开路电压约为1V。制备的三节串联电堆以加湿氢气为燃料800°C最大功率输出为2.8W，以加湿甲烷为燃料时电堆在800°C和850°C的最大输出功率分别达到3.0W和4.0W，说明采用凝胶注模成型工艺制备的电池性能较好。电堆在850°C以甲烷为燃料10mA/cm~2的恒电流密度下放电4.5h后电堆的性能下降，因此寻找抗积碳的新型阳极使SOFC在碳氢化合物中稳定运行是非常必要的。
本论文开发了一种新型阳极材料(Ni_(0.75)Fe_(0.25)-5MgO)/YSZ。通过对合成的Ni_(0.75)Fe_(0.25)O粉体进行XRD表征发现， Fe已经进入了NiO的立方晶格，形成了Ni_(0.75)Fe_(0.25)O固溶体。研究了MgO的掺杂量对SOFC性能的影响，结果表明，阳极中加入一定量的Fe和MgO后，电池的最大功率密度增大，但加入过多的MgO其性能反而下降。以(Ni_(0.75)Fe_(0.25)-5MgO)/YSZ为阳极的SOFC使用加湿甲烷为燃料时800°C的最大输出功率达到648mW/cm~2，确定了MgO的最佳掺杂量为5wt.%。不同阳极的SOFC的恒电流放电曲线表明，以Ni0.75Fe0.25/YSZ为阳极的SOFC在甲烷中很快衰减，当阳极中加入一定量的MgO后，电压在整个20h的测试过程中保持相对稳定。原因可能是阳极中加入一定量的稳定金属氧化物MgO可以抑制碳纤维的生长，或者使得YSZ骨架有足够的机械强度来承受由于碳纤维的生长对其产生的应力。对各电池经稳定性测试后阳极SEM图的分析结果进一步证实了上述机理推测。本章充分证明了(Ni0.75Fe0.25–5MgO)/YSZ阳极在直接使用甲烷为燃料的锥管状固体氧化物燃料电池中应用的可行性。
在上述研究工作的基础上，研究了以(Ni_(0.75)Fe_(0.25)-5MgO)/YSZ为阳极的SOFC直接使用CO为燃料的性能。结果表明，以H2为燃料的电池性能都要高于以CO为燃料的性能，而以干燥CO为燃料的电池性能都要高于以加湿CO为燃料的性能。稳定性测试表明，以(Ni_(0.75)Fe_(0.25)-5MgO)/YSZ为阳极的单电池在800°C以83mA/cm~2的恒电流测试的40h内电压都相当稳定，而以Ni/YSZ为阳极的单电池工作了10h后电压快速下降为零，并且水对以(Ni_(0.75)Fe_(0.25)-5MgO)/YSZ为阳极的单电池使用CO为燃料时的稳定性没有影响。SEM测试结果表明，使用CO为燃料时，在Ni/YSZ阳极表面的积碳比(Ni_(0.75)Fe_(0.25)-5MgO)/YSZ阳极的严重。制备的两节串联电堆使用加湿CO为燃料时，在800°C的开路电压和最大输出分别为2V和4W，电堆在以83mA/cm~2的恒电流密度下放电的90h内表现出良好的稳定性，进一步证明(Ni_(0.75)Fe_(0.25)-5MgO)/YSZ新型阳极非常适合于固体氧化物燃料电池使用含碳燃料的便携式应用。
本论文设计并开发了一种适合于直接碳固体氧化物燃料电池便携式应用的装置。证明了碳燃料中加入适量的FemOn能催化炭的Boudouard反应，提高电池性能。以担载5wt.%Fe催化剂的活性炭为燃料，制备的便携式DC-SOFC单电池850°C的开路电压达1.05V，最大功率密度达到280mW/cm~2。寿命测试结果表明，电池以小电流放电时，电压维持较稳定，随着运行电流的增大，电池的寿命减小。小电流放电后容器内剩余的红褐色粉末经EDX测试分析主要为铁的氧化物，表明炭已消耗完。制备的便携式三节串联DC-SOFC电池组使用担载5wt.%Fe的活性炭为燃料时电化学性能较低。这是由于该便携式装置的密封难度大，如何解决该装置的密封问题也是今后我们工作的重点。
Solid oxide fuel cell (SOFC) is a highly efficient, environment friendly and all-solid-state electrochemical power generation device, which uses a solid ceramic material as theelectrolyte and has a wide range of applications. The cone-shaped tubular segmented-in-seriesSOFC design can achieve a relatively higher voltage and power in a limited space, goodthermal shock resistance and thermal cycling capability, so that it is specially suitable forSOFC stack for portable applications, which need light weight and compact volume. Thisthesis centers around the research and development of technique to frabricate cone-shapedtubular SOFC, new anode material and its anti-coking mechanism, a novel direct carbon solidoxide fuel cell (DC-SOFC) device to speed up the industrialization process of cone-shapedtubular SOFC for portable application.
Gel-casting technique is developed to fabricate the green cone-shaped anode substratesand the performance of a single cell and stack are investigated. The results show that themicrostructure of the cell fabricated by gel-casting technique is ideal, YSZ electrolyte filmfabricated by co-sintering of the electrolyte and green anode substrates is dense and adhereswell to both the anode and cathode. The maximum power density of the single cell usinghydrogen as fuel is about600and900mW/cm~2at750°C and800°C, respectively. The opencircuit voltage (OCV) is about1V. The maximum output power of the three-cell-stack usinghydrogen as fuel is about2.8W. When using methane as fuel, the maximum output power is3.0and4.0W at800°C and850°C. It means that the performance of the cell fabricated bygel-casting technique is fine. The performance of the stack decreases when measured under aconstant current density of10mA/cm~2at850°C using humidified methane as fuel. So findingnew anode material with anti-coking ability for SOFC using hydrocarbons as fuel isimperative.
A new anode material (Ni_(0.75)Fe_(0.25)-5MgO)/YSZ is developed. The X-ray spectrum of thefabricated Ni_(0.75)Fe_(0.25)O power indicats that Fe was doped into the crystal structure of NiO,forming a solid Ni1xFexO solution. The results show that the power density increases as aproper amount of Fe and MgO is doped into the anode, while the performance decreases astoo much MgO is added into the anode. A maximum power density of648mW/cm~2at0.7Vand800°C for the SOFC with (Ni_(0.75)Fe_(0.25)-5MgO)/YSZ anode is achieved using humidifiedmethane as fuel. The stability test results for the cells with different anodes show that the cellwith Ni0.75Fe0.25/YSZ anode fails rapidly in methane. When MgO is added into the bulk anode,the voltage remains stable over the whole period of20h. This may be explaned as follows: on the one hand, the doped stable oxide MgO can suppress carbon fiber growth; on the otherhand, MgO particles located on the grain boundaries of YSZ make the YSZ skeleton strongenough to stand the stress caused by carbon fiber growth. SEM micrographs of the anodesubstrates of the single cells after the output performance and stability test further strengthenthe mechanisms above. This proves that (Ni0.75Fe0.25–5MgO)/YSZ is a promising anodematerial for cone-shaped tubular SOFCs operated on methane fuel.
Based on the works above, we have researched on the performance of SOFCs with(Ni_(0.75)Fe_(0.25)-5MgO)/YSZ anode using CO as fuel. For the cell with either of the anodes, theperformance on hydrogen is better than that on CO, and that on moist CO is poorer than ondry CO. The durability results show that while the cells with traditional Ni/YSZ anode failafter operating on either dry or moist CO for about10h, the voltage of the cells with(Ni_(0.75)Fe_(0.25)-5MgO)/YSZ anode remains stable during the whole test time (40h). And thepresence of water in CO fuel has no effect on the stability of cell with (Ni0.75Fe0.25-5%MgO)/YSZ anode. SEM images of the surface of the anodes after output performance andstability test shows that cells with Ni/YSZ anodes have more deposition than (Ni0.75Fe0.25-5MgO)/YSZ anode when using CO as fuel. The OCV of the two-cell-stack with (Ni0.75Fe0.25-5MgO)/YSZ anode is2V and its maximum output power is4W at800°C. A durability testof the two-cell-stack on moist CO is performed at a constant current density of83mAcm2. Itindicates that the stability of the as-prepared two-cell-stack with (Ni_(0.75)Fe_(0.25)-5MgO)/YSZanode is good during the whole testing time of90h. This character is very significant for theportable application of SOFCs operated on carbon fuel.
A portable device has been designed for the application of direct carbon solid oxide fuelcell. The results show that Fe catalyst catalyses the Boudouard reaction of cabon fuel andimproves the cell performance. The OCV of the single DC-SOFC is1.05V and its maximumoutput power density is280mW/cm~2at850°C. Stability test results show that the voltage canremain stable when the operating current is small and larger operating current resulted inshorter operation life. EDX analysis shows that the reddish fuel residue is mainly Fe2O3andindicates carbon fuel is depleted. The performance of the three-cell DC-SOFC stack forportable application is poor. For sealing is difficult for this portable device, further work isnecessary to solve the sealing problems of this portable device.
引文
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