多孔阳极支撑中温固体氧化物燃料电池的制备及性能研究
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摘要
固体氧化物燃料电池(SOFC)是一种把燃料的化学能直接转化为电能的全固态装置,在环境友好和能源高效利用方面显示出明显的优势,受到越来越多的关注。当前固体氧化物燃料电池发展的一个趋势是将其工作温度中低温化(工作温度在800℃以下)。为保证电池具有良好的输出性能,采用高电导率的电解质材料(La0.9Sr0.1Ga0.8Mg0.2O3-δ (LSGM)和电解质层薄膜化技术是一种非常有前景的技术路线。
本文采用多孔阳极材料作为支撑体,应用电解质层薄膜化技术制备单电池片。先采用甘氨酸-硝酸盐法(Glycine-Nitrate Process, GNP)合成了La0.7Sr0.3Cr0.5Mn0.5O3-δ(LSCM)阳极粉末和La0.4Ce0.6O2-δ(LDC)粉末。采用Materials Studio软件计算模拟了LSCM材料的晶体结构,键长和态密度等。并把LSCM阳极粉末分别与三种不同种类和含量的造孔剂混合后,在5种不同制片压力下制备多孔阳极片。8wt.%淀粉造孔剂,造孔效果最好,制片压力为10MPa时,阳极片最大孔隙率为45%,比表面积达到1.256g/cm2。所制备的LDC粉末与不同含量的NiO混合制备复合阳极材料,加入造孔剂后在135℃烧结后得到颗粒接触较好的多孔阳极片,当NiO与LDC粉末比例为5：5时,NiO-LDC阳极片的孔隙率为30%左右,此时在800℃电导率最大。
接下来分别在LSCM多孔阳极基底和NiO-LDC多孔阳极基底上采用射频磁控溅射法和浆料旋涂法制备了LSGM薄膜。并分别探讨了射频磁控溅射法和浆料旋涂法制备LSGM电解质薄膜的工艺参数。得出磁控溅射法沉积LSGM电解质薄膜的最佳工艺参数为：溅射压强为5Pa,射频功率为210W,基底温度为300℃,退火温度为1000℃,退火时间为2h。采用优化后的工艺参数获得的LSGM薄膜,致密度高,结晶性好,与阳极基底结合紧密。研究发现,沉积基底温度越高,LSGM电解质薄膜的沉积速率越小,薄膜材料颗粒越大。同时探索了LSGM薄膜沉积机理,分别采用lmin、3min和5min在单晶硅片上沉积LSGM电解质薄膜。研究表明,LSGM电解质薄膜沉积呈岛状生长模式,并呈择优生长现象,经退火后,不均匀现象和择优生长现象均消失。浆料旋涂法制备LSGM电解质薄膜研究结果表明,采用5wt.%乙基纤维素和5wt.%松油醇分别作为粘结剂和调和剂制备LSGM电解质浆料,经过重复旋涂9层后,在1400℃烧结4h,可以制备得到致密的LSGM电解质层。
为了研究LSGM电解质材料中O2-传导过程,采用Materials Studio软件计算模拟LSGM晶体结构、键长和态密度等,并模拟了LSGM电解质材料中O2-传导的分子动力学过程。研究发现,LSGM晶体中与Ga和Mg成键的O2-很容易发生迁移,参与晶体中O2-的传导,并从过渡态计算中分析O2-迁移能,Sr和Mg掺杂后与Ga利Mg成键的O2-的迁移能分别为-0.152eV和-0.232eV,有利于晶体中与Ga和Mg成键的O2-传导,参与电化学反应。
最后在LSCM和NiO-LDC阳极基底上,分别采用磁控溅射法和浆料旋涂法制备了4种不同体系的单电池片,并对单电池片截面形貌、交流阻抗、开路电压和功率密度进行了分析。研究表明,磁控溅射法制备的LSGM电解质层致密均匀,与基底粘结性好,单电池片的交流阻抗较小,尤其是在NiO-LDC体系单电池中,磁控溅射法制备的单电池在750℃的极化阻抗和欧姆阻抗分别为0.14Ω·cm2和0.74Ω·cm2,而浆料旋涂法制备单电池的极化阻抗和欧姆阻抗分别为3.23Ω·m2和1.81Ω·cm2,相差较大。研究还发现,不管是LSCM多孔阳极基底还是NiO-LDC多孔阳极基底单电池,磁控溅射法制备的单电池极化阻抗小于欧姆阻抗,而浆料旋涂法制备单电池极化阻抗大于欧姆阻抗。LSCM(支撑体)/LSGM/LSCF单电池片的开路电压(OCV)较高,最大达到1.09V,接近理论值。而NiO-LDC (支撑体)/LSGM/LSCF单电池片的OCV较低,高温时只有0.7V左右,而NiO-LDC (支撑体)/LSGM/LSCF单电池片的最大电流密度和功率密度较好。在NiO-LDC(支撑体)/LSGM/LSCF单电池片体系中磁控溅射法和浆料旋涂法制备单电池片的最大电流密度和功率密度分别为700℃的370.71mA/cm2,71.23mW/cm2和750℃的290.72mA/cm2,44.12mW/cm2。相比较而言,磁控溅射法制备的单电池的结构和性能优于浆料旋涂法制备的单电池。
Solid oxide fuel cell (SOFC), which is an all solid device to convert the chemical energy of the fuel into electrical energy directly, has been played great attention duo to high efficiency and environmental protection. Currently, the development tendency for SOFC is lower the operating temperature (the operating temperature below800℃). In order to obtain the excellent output performance, employing an electrolyte material with high conductivity (La0.9Sr0.1Ga0.8Mg0.2O3-δ (LSGM)) and the technologies for electrolyte layer to be film is a very promising technology route.
In this paper, the single cells were supported by porous anode substrates, and the electrolyte layers were prepared to be film by the film-technologies. Firstly. La0.7Sr0.3Cr0.5Mn0.5O3-δ (LSCM) anode powder and La0.4Ce0.6O2-δ(LDC) powder were synthesized by glycine nitrate process (GNP). And the LSCM crystal structure, bond length and density of states (DOS) were simulated by Materials Studio software. And the LSCM anode powder mixed with three types of pore-formers with different amounts, the mixtures were pressed into pellets by five pressures.8wt.%starch as the pore-former has the best the capability for porosity, when the pressure at10MPa, the maximum porosity of the anode was45%. LDC powders and NiO powders was mixed to be composite anode materials with different ratios, after mixing with pore formers, the mixtures were sintered to form pore anode pellets, and the particles of the anode materials were very well. When the ratio of LDC and NiO was5:5, the porosity was about30%, and the conductivity of the anode pellet was the highest at800℃
Next, the LSGM electrolyte films were prepared by radio frequency magnetron sputtering and slurry spin coating on LSCM and NiO-LDC porous anode substrate, respectively, and the parameters of the preparing films were explored. In the sputtering process for LSGM film, the substrate temperature. Ar pressure and depositing power for the film were explored, and the optimum process parameters for the film deposited by magnetron sputtering:sputtering pressure is5Pa, depositing power is210W, substrate temperature is300℃, annealing temperature is1000℃, annealing time is2h. Depositing with the optimized process parameters. LSGM film was very dense, the crystallinity of the film was very good, and the film adhered to the substrate closely. The study illustrated that the deposited rate becomes less and the particle size of the film become greater when the substrate temperature was higher.
The deposited mechanism was also discussed. The film was deposited on Si pellets in1,3and5min, respectively. The research showed that LSGM electrolyte film was deposited with island growth mode, and the film appeared phenomenon of preferential growth. After annealing, the phenomenon of preferential growth and the uneven film were disappeared. The results of slurry spin coating showed that a dense film can be obtained by employing the process parameters:5wt.%Ethyl cellulose as a binder.5wt.%Terpineol as moderator agent repeating spin9times and sintering at1400℃for4h.
In order to research the process of O2-conduction in LSGM crystal, the LSGM crystal structure, bond length and density of state were calculated and simulated by the Materials Studio software, and the transfer process dynamics of O2-in LSGM crystal was also simulated. The research found that the O2-which formed bond with Ga/Mg in La90Sr10Ga80Mg20O287crystal was very easy to transfer. The transfer energy of the O2-was also calculated though analysis of the transition process. The transfer energies of the O2" which formed bond with Ga and Mg were-0.152eV and-0.232eV, respectively, which was benefit to the transfer of O2-
Finally, the LSGM electrolyte layer were fabricated by magnetron sputtering and slurry spin coating on LSCM or NiO-LDC anode substrate, and four kinds of single cells were prepared, and the cross-sectional morphologies, AC impedance, open circuit voltage (OCV) and power density of the cells were explored. The studies illustrated that the film prepared by magnetron sputtering was dense and uniform, adhered to anode substrates closely, and the AC impedance of the single cell was small, especially for the single cell of NiO-LDC/LSGM/LSCF. If the cell prepared by sputtering, the polarization resistivty and ohmic resistivity of the single cell prepared by magnetron sputtering were0.14Ω·cm2and0.74Ω·cm2respectively. And the polarization resistivty and ohmic resistivity of the single cell prepared by spin coating were3.23Ω·cm2and1.8Ω·cm2respectively. Regardless of the LSCM or NiO-LDC porous anode substate. the polarization resistivity of the cell prepared by magnetron sputtering was less than the ohmic resistivity of it, however the polarization resistivity of the cell prepared by spin coating was larger than the ohmic resistivity of it.
The open circuit voltage of the LSCM (supported)/LSGM/LSCF single cell was great, and the maximum was1.09V, which was very close to the theoretical value. The open circuit voltage of NiO-LDC (supported)/LSGM/LSCF single cell was small, the OCV at high temperature was about0.7V, however, the largest current and largest power of the NiO-LDC (supported)/LSGM/LSCF single cell were very well. The largest current density and power density of the single cells prepared by magnetron sputtering and slurry spin coating were370.71mA/cm2,71.23mW/cm2and290.72mA/cm2,44.12mW/cm2, respectively. In a word, the structure and performance of the single cell prepared by magnetron sputtering are better than those prepared by slurry spin coating.
本文采用多孔阳极材料作为支撑体,应用电解质层薄膜化技术制备单电池片。先采用甘氨酸-硝酸盐法(Glycine-Nitrate Process, GNP)合成了La0.7Sr0.3Cr0.5Mn0.5O3-δ(LSCM)阳极粉末和La0.4Ce0.6O2-δ(LDC)粉末。采用Materials Studio软件计算模拟了LSCM材料的晶体结构,键长和态密度等。并把LSCM阳极粉末分别与三种不同种类和含量的造孔剂混合后,在5种不同制片压力下制备多孔阳极片。8wt.%淀粉造孔剂,造孔效果最好,制片压力为10MPa时,阳极片最大孔隙率为45%,比表面积达到1.256g/cm2。所制备的LDC粉末与不同含量的NiO混合制备复合阳极材料,加入造孔剂后在135℃烧结后得到颗粒接触较好的多孔阳极片,当NiO与LDC粉末比例为5：5时,NiO-LDC阳极片的孔隙率为30%左右,此时在800℃电导率最大。
接下来分别在LSCM多孔阳极基底和NiO-LDC多孔阳极基底上采用射频磁控溅射法和浆料旋涂法制备了LSGM薄膜。并分别探讨了射频磁控溅射法和浆料旋涂法制备LSGM电解质薄膜的工艺参数。得出磁控溅射法沉积LSGM电解质薄膜的最佳工艺参数为：溅射压强为5Pa,射频功率为210W,基底温度为300℃,退火温度为1000℃,退火时间为2h。采用优化后的工艺参数获得的LSGM薄膜,致密度高,结晶性好,与阳极基底结合紧密。研究发现,沉积基底温度越高,LSGM电解质薄膜的沉积速率越小,薄膜材料颗粒越大。同时探索了LSGM薄膜沉积机理,分别采用lmin、3min和5min在单晶硅片上沉积LSGM电解质薄膜。研究表明,LSGM电解质薄膜沉积呈岛状生长模式,并呈择优生长现象,经退火后,不均匀现象和择优生长现象均消失。浆料旋涂法制备LSGM电解质薄膜研究结果表明,采用5wt.%乙基纤维素和5wt.%松油醇分别作为粘结剂和调和剂制备LSGM电解质浆料,经过重复旋涂9层后,在1400℃烧结4h,可以制备得到致密的LSGM电解质层。
为了研究LSGM电解质材料中O2-传导过程,采用Materials Studio软件计算模拟LSGM晶体结构、键长和态密度等,并模拟了LSGM电解质材料中O2-传导的分子动力学过程。研究发现,LSGM晶体中与Ga和Mg成键的O2-很容易发生迁移,参与晶体中O2-的传导,并从过渡态计算中分析O2-迁移能,Sr和Mg掺杂后与Ga利Mg成键的O2-的迁移能分别为-0.152eV和-0.232eV,有利于晶体中与Ga和Mg成键的O2-传导,参与电化学反应。
最后在LSCM和NiO-LDC阳极基底上,分别采用磁控溅射法和浆料旋涂法制备了4种不同体系的单电池片,并对单电池片截面形貌、交流阻抗、开路电压和功率密度进行了分析。研究表明,磁控溅射法制备的LSGM电解质层致密均匀,与基底粘结性好,单电池片的交流阻抗较小,尤其是在NiO-LDC体系单电池中,磁控溅射法制备的单电池在750℃的极化阻抗和欧姆阻抗分别为0.14Ω·cm2和0.74Ω·cm2,而浆料旋涂法制备单电池的极化阻抗和欧姆阻抗分别为3.23Ω·m2和1.81Ω·cm2,相差较大。研究还发现,不管是LSCM多孔阳极基底还是NiO-LDC多孔阳极基底单电池,磁控溅射法制备的单电池极化阻抗小于欧姆阻抗,而浆料旋涂法制备单电池极化阻抗大于欧姆阻抗。LSCM(支撑体)/LSGM/LSCF单电池片的开路电压(OCV)较高,最大达到1.09V,接近理论值。而NiO-LDC (支撑体)/LSGM/LSCF单电池片的OCV较低,高温时只有0.7V左右,而NiO-LDC (支撑体)/LSGM/LSCF单电池片的最大电流密度和功率密度较好。在NiO-LDC(支撑体)/LSGM/LSCF单电池片体系中磁控溅射法和浆料旋涂法制备单电池片的最大电流密度和功率密度分别为700℃的370.71mA/cm2,71.23mW/cm2和750℃的290.72mA/cm2,44.12mW/cm2。相比较而言,磁控溅射法制备的单电池的结构和性能优于浆料旋涂法制备的单电池。
Solid oxide fuel cell (SOFC), which is an all solid device to convert the chemical energy of the fuel into electrical energy directly, has been played great attention duo to high efficiency and environmental protection. Currently, the development tendency for SOFC is lower the operating temperature (the operating temperature below800℃). In order to obtain the excellent output performance, employing an electrolyte material with high conductivity (La0.9Sr0.1Ga0.8Mg0.2O3-δ (LSGM)) and the technologies for electrolyte layer to be film is a very promising technology route.
In this paper, the single cells were supported by porous anode substrates, and the electrolyte layers were prepared to be film by the film-technologies. Firstly. La0.7Sr0.3Cr0.5Mn0.5O3-δ (LSCM) anode powder and La0.4Ce0.6O2-δ(LDC) powder were synthesized by glycine nitrate process (GNP). And the LSCM crystal structure, bond length and density of states (DOS) were simulated by Materials Studio software. And the LSCM anode powder mixed with three types of pore-formers with different amounts, the mixtures were pressed into pellets by five pressures.8wt.%starch as the pore-former has the best the capability for porosity, when the pressure at10MPa, the maximum porosity of the anode was45%. LDC powders and NiO powders was mixed to be composite anode materials with different ratios, after mixing with pore formers, the mixtures were sintered to form pore anode pellets, and the particles of the anode materials were very well. When the ratio of LDC and NiO was5:5, the porosity was about30%, and the conductivity of the anode pellet was the highest at800℃
Next, the LSGM electrolyte films were prepared by radio frequency magnetron sputtering and slurry spin coating on LSCM and NiO-LDC porous anode substrate, respectively, and the parameters of the preparing films were explored. In the sputtering process for LSGM film, the substrate temperature. Ar pressure and depositing power for the film were explored, and the optimum process parameters for the film deposited by magnetron sputtering:sputtering pressure is5Pa, depositing power is210W, substrate temperature is300℃, annealing temperature is1000℃, annealing time is2h. Depositing with the optimized process parameters. LSGM film was very dense, the crystallinity of the film was very good, and the film adhered to the substrate closely. The study illustrated that the deposited rate becomes less and the particle size of the film become greater when the substrate temperature was higher.
The deposited mechanism was also discussed. The film was deposited on Si pellets in1,3and5min, respectively. The research showed that LSGM electrolyte film was deposited with island growth mode, and the film appeared phenomenon of preferential growth. After annealing, the phenomenon of preferential growth and the uneven film were disappeared. The results of slurry spin coating showed that a dense film can be obtained by employing the process parameters:5wt.%Ethyl cellulose as a binder.5wt.%Terpineol as moderator agent repeating spin9times and sintering at1400℃for4h.
In order to research the process of O2-conduction in LSGM crystal, the LSGM crystal structure, bond length and density of state were calculated and simulated by the Materials Studio software, and the transfer process dynamics of O2-in LSGM crystal was also simulated. The research found that the O2-which formed bond with Ga/Mg in La90Sr10Ga80Mg20O287crystal was very easy to transfer. The transfer energy of the O2-was also calculated though analysis of the transition process. The transfer energies of the O2" which formed bond with Ga and Mg were-0.152eV and-0.232eV, respectively, which was benefit to the transfer of O2-
Finally, the LSGM electrolyte layer were fabricated by magnetron sputtering and slurry spin coating on LSCM or NiO-LDC anode substrate, and four kinds of single cells were prepared, and the cross-sectional morphologies, AC impedance, open circuit voltage (OCV) and power density of the cells were explored. The studies illustrated that the film prepared by magnetron sputtering was dense and uniform, adhered to anode substrates closely, and the AC impedance of the single cell was small, especially for the single cell of NiO-LDC/LSGM/LSCF. If the cell prepared by sputtering, the polarization resistivty and ohmic resistivity of the single cell prepared by magnetron sputtering were0.14Ω·cm2and0.74Ω·cm2respectively. And the polarization resistivty and ohmic resistivity of the single cell prepared by spin coating were3.23Ω·cm2and1.8Ω·cm2respectively. Regardless of the LSCM or NiO-LDC porous anode substate. the polarization resistivity of the cell prepared by magnetron sputtering was less than the ohmic resistivity of it, however the polarization resistivity of the cell prepared by spin coating was larger than the ohmic resistivity of it.
The open circuit voltage of the LSCM (supported)/LSGM/LSCF single cell was great, and the maximum was1.09V, which was very close to the theoretical value. The open circuit voltage of NiO-LDC (supported)/LSGM/LSCF single cell was small, the OCV at high temperature was about0.7V, however, the largest current and largest power of the NiO-LDC (supported)/LSGM/LSCF single cell were very well. The largest current density and power density of the single cells prepared by magnetron sputtering and slurry spin coating were370.71mA/cm2,71.23mW/cm2and290.72mA/cm2,44.12mW/cm2, respectively. In a word, the structure and performance of the single cell prepared by magnetron sputtering are better than those prepared by slurry spin coating.
引文
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