平板式中温SOFC阳极系统的研究
摘要
固体氧化物燃料电池(Solid Oxide Fuel Cells, SOFCs)具有全固态、高效率等优点,能量转换效率最高可达80%,是目前世界各个国家的研究热点之一。这种电池阳极与电解质通常共烧结在一起。为了防止高温下氧化气与还原气混合而发生爆炸,需要将还原性气体与氧化性气体用密封材料隔离。
研究了具有链状结构的淀粉和具有球形结构的聚甲基丙烯酸甲脂(PMMA`)作为阳极支撑层造孔剂,实验结果发现,15mass%淀粉制备的阳极孔隙率为29.8%,电导率为2000.35S·cm~(-1);而15mass%和30mass%PMMA制备的阳极孔隙率分别是36.4%和59.4%,电导率分别是1200.0S·cm~(-1)和1008.45S·cm~(-1)。制备的电池放电测试表明,当孔隙率小于59.4%时,相同H2流速下电池的功率密度随孔隙率的增加而增加;当孔隙率达到59.4%时,H2流速的增加对电池功率密度的提高影响不明显。
用平均粒径大于1μm的NiO-Ⅰ、NiO-Ⅱ和NiO-Ⅲ用于制备阳极功能层,发现NiO-Ⅰ制备的电池的放电功率密度最高,达到121 mW·cm~(-2),而NiO-Ⅲ制备的电池功率密度仅有81 mW·cm~(-2),SEM分析表明NiO-Ⅰ的颗粒比较细小,平均粒径约2μm,而NiO-Ⅲ达到4.47μm;采用沉淀法制备的纳米NiO-Ⅳ和商品纳米NiO-Ⅴ制备的电池,最大功率密度分别高达205.3 mW·cm~(-2)和308.2 mW·cm~(-2),原因在于纳米颗粒尺寸小,比表面积大,催化性好,与YSZ的附着性佳。700℃煅烧增加了NiO-Ⅴ的活性,电池功率密度增加到369.0 mW·cm~(-2)。对阳极功能层的YSZ在1200℃煅烧后再球磨12h,电池最大功率密度达到了390.5 mW·cm~(-2),原因是锻烧球磨的YSZ呈球形,增加了NiO分散的均匀性。
对于目前国内普遍作为SOFC电解质使用的JC 8YSZ和TOSOH 8YSZ进行实验比较。实验表明两者都是在1000℃开始发生收缩,JC 8YSZ的最大收缩率为25.2%,而TOSOH 8YSZ的最大收缩率只有19.0%。TOSOH 8YSZ的平均粒径为0.71μm,JC 8YSZ的平均粒径为1.91μm。测试的Nyquist曲线表明在800℃时JC 8YSZ和TOSOH 8YSZ的电导率分别是0.0179S·cm~(-1)和0.0212 S·cm~(-1),计算活化能分别是108.35kJ·mol~(-1)和105.67 kJ·mol~(-1),用这两种8YSZ制备的电池在800℃最大功率密度分别是184.08 mW·cm~(-2)和267.75 mW·cm~(-2)。SEM照片表明两种8YSZ在1500℃烧结时都不致密,但是采用80%JC与20%TOSOH 8YSZ混合则可以得到致密的电解质膜。厚度20μm时,开路电压800℃可达1002mV,放电功率密度447.0 mW·cm~(-2),并且保持稳定,而当厚度降低到7μm时,开路电压800℃只有923mV,放电功率密度253mW·cm~(-2),并且开路电压在20min内降低,原因是还原过程阳极体积的变化导致电解质破裂。
SLABS3与SOFC组元共烧时粘接性良好。能谱分析表明,向微晶玻璃方向,与NiO/YSZ阳极共烧Zr的扩散深度10μm;与阴极共烧Mn的扩散深度60μm;与连接体共烧,Cr和Fe的扩散深度约20μm,但是微晶玻璃的成分却没有向相邻组元扩散,符合兼容性要求。制备的模拟电池用该密封材料隔离H2和O2,开路电压热循环6次仍保持在1.05V左右,表明SLABS3密封的模拟电池的气密性和稳定性良好。
由于硬密封导致电池无法拆卸,同时研究了云母和气相SiO2填充的陶瓷纤维作为压实密封材料。结果表明,采用气相SiO2填充的陶瓷纤维的泄漏率随气相SiO2填充量的增加而减小。填充的陶瓷纤维预压后在1MPa压力,10kPa气压差下泄漏率仅为0.04sccm·cm~(-1),密封性能优于云母,该泄漏率值低于文献报道水平,达到国际先进水平,并且热循环20次保持稳定,在800℃下H2还原200h质量损失速率为1.7×10~(-2)g·cm~(-2)·h~(-1),还原后不影响泄漏率。
Solid oxide fuel cell (SOFC) has the advantage of all solid component and high conversion efficiency, which is as high as 80%, so it is one of the focus study in the world. Normally the anode electrode and electrolyte were co-sintered together. To prevent the mixture of oxygen and hydrogen at high temperature, seals, which were pasted on anode electrode, were required.
Line structure of starch and ball structure of polymethyl methacrylate( PMMA) as pore-formers for SOFC anode supported layer were compared. The results demonstrated that the the porosity was 29.8%, electronic conductivity was 2000.35S·cm~(-1) for 15mass% starch as pore-formers. But the porosity was 36.4% and 59.4%, and conductivity was 1200.0 S·cm~(-1) and 1008.45 S·cm~(-1) respectively for 15mass% and 30mass% PMMA pore-formers.
Discharging curvess for the cell prepared by different pore-formers and their contents demonstrated that when the porosity is lower than 59.4%, the Discharging property increased with the porosity, but the influence of H2 flow rate on Discharging curve is not obvious when the porosity is 59.4%. Three average particle sizes higher than 1μm of NiO were studied as anode functional layer. The cell performance is the highest for the cell prepared NiO-,with the maxium powder density 121 mW·cm~(-2) ,but only 81 mW·cm~(-2) for NiO-.Scanning electron microscope (SEM) images showed that the particle size of NiO-Ⅰwas about 2μm, but 4.47μm for NiO-Ⅲ.To reduce the NiO particle size, nano NiO-Ⅳproduced by co-precipitation and commercial NiO-Ⅴwere used as SOFC anode functional layer. The maximum power density of the cell was 205.3mW·cm~(-2) and 308.2mW·cm~(-2) respectively, and the cell power density prepared from NiO-Ⅴcalcined at 700℃increased to 369.0mW·cm~(-2) .YSZ coarsened at 1200℃and milled for 12h let the cell power density increase to 390.5mW·cm~(-2).
Dimension of JC 8YSZ and TOSOH 8YSZ ,which were widely used as SOFC electrolye, were measured. The results showed that they shrinked at 1000℃. The total shrinkage of JC YSZ was 25.2%, but that of TOSOH 8YSZ was 19.0%. Particle analysis showed that the average particle size of TOSOH 8YSZ was 0.71μm, only about 2.5fold of that JC 8YSZ, which was 1.91μm. The electrochemical analynis demonstrated that the electronic donductivity of JC 8YSZ and TOSOH 8YSZ at 800℃were 0.0179S·cm~(-1) and 0.0212 S·cm~(-1) respectively. The calculated activation energies were 108.35kJ·mol~(-1) and 105.67kJ·mol~(-1) respectively. The maximum powder density of the cells made up of these two 8YSZ at 800℃were 184.08 mW·cm~(-2) for JC 8YSZ and 267.75 mW·cm~(-2) for TOSOH 8YSZ. SEM images showed that none of the electrolyte made of this two YSZ was dense, but was denser made of 80%JC YSZ and 20%TOSOH YSZ mixture. When the thickness of the electrolyte was 20μm, the open current voltage of the electrolyte was 1002mV and its power density reached 447mW·cm~(-2) while kept stable. However, when the thickness reduced to 13μm, there was only 253mW·cm~(-2) for the power density, and 923mV for the OCV, and decreased in 20min. The reason was that the voltage change during anode reduction led to YSZ electrolyte crack.
SLABS3 ceramic glass“glue”SOFC other components well. During co-calcined for 100h, Zr element diffused 10μm to glass, Mn with 60μm , Cr and Fe element about 20μm, but none element of the glass would diffuse to SOFC other components, which meet the requirement of compatibility.The OCV test remained higher than 1.05V,demonstrating that seals meet the requirement in 6 circles.
However, as the solid seals cause the problem of stack unable replacement, so compressive seals were also studied. Leakage test for alumina silica infiltrated ceramic fiber paper and mica were studied. The results demonstrated that the leakage of the infiltrated ceramic fiber paper was 0.04sccm·cm~(-1), which was lower than that of mica. This value is lower than the leakage reported. The infiltrated ceramic fiber paper were stabe in 20 thermal cycles and the weight loss at 800℃under hydrogen atmosphere was 1.7×10~(-2)g·cm~(-2)·h~(-1) for 200h, which showed no effect on sealing performance.
研究了具有链状结构的淀粉和具有球形结构的聚甲基丙烯酸甲脂(PMMA`)作为阳极支撑层造孔剂,实验结果发现,15mass%淀粉制备的阳极孔隙率为29.8%,电导率为2000.35S·cm~(-1);而15mass%和30mass%PMMA制备的阳极孔隙率分别是36.4%和59.4%,电导率分别是1200.0S·cm~(-1)和1008.45S·cm~(-1)。制备的电池放电测试表明,当孔隙率小于59.4%时,相同H2流速下电池的功率密度随孔隙率的增加而增加;当孔隙率达到59.4%时,H2流速的增加对电池功率密度的提高影响不明显。
用平均粒径大于1μm的NiO-Ⅰ、NiO-Ⅱ和NiO-Ⅲ用于制备阳极功能层,发现NiO-Ⅰ制备的电池的放电功率密度最高,达到121 mW·cm~(-2),而NiO-Ⅲ制备的电池功率密度仅有81 mW·cm~(-2),SEM分析表明NiO-Ⅰ的颗粒比较细小,平均粒径约2μm,而NiO-Ⅲ达到4.47μm;采用沉淀法制备的纳米NiO-Ⅳ和商品纳米NiO-Ⅴ制备的电池,最大功率密度分别高达205.3 mW·cm~(-2)和308.2 mW·cm~(-2),原因在于纳米颗粒尺寸小,比表面积大,催化性好,与YSZ的附着性佳。700℃煅烧增加了NiO-Ⅴ的活性,电池功率密度增加到369.0 mW·cm~(-2)。对阳极功能层的YSZ在1200℃煅烧后再球磨12h,电池最大功率密度达到了390.5 mW·cm~(-2),原因是锻烧球磨的YSZ呈球形,增加了NiO分散的均匀性。
对于目前国内普遍作为SOFC电解质使用的JC 8YSZ和TOSOH 8YSZ进行实验比较。实验表明两者都是在1000℃开始发生收缩,JC 8YSZ的最大收缩率为25.2%,而TOSOH 8YSZ的最大收缩率只有19.0%。TOSOH 8YSZ的平均粒径为0.71μm,JC 8YSZ的平均粒径为1.91μm。测试的Nyquist曲线表明在800℃时JC 8YSZ和TOSOH 8YSZ的电导率分别是0.0179S·cm~(-1)和0.0212 S·cm~(-1),计算活化能分别是108.35kJ·mol~(-1)和105.67 kJ·mol~(-1),用这两种8YSZ制备的电池在800℃最大功率密度分别是184.08 mW·cm~(-2)和267.75 mW·cm~(-2)。SEM照片表明两种8YSZ在1500℃烧结时都不致密,但是采用80%JC与20%TOSOH 8YSZ混合则可以得到致密的电解质膜。厚度20μm时,开路电压800℃可达1002mV,放电功率密度447.0 mW·cm~(-2),并且保持稳定,而当厚度降低到7μm时,开路电压800℃只有923mV,放电功率密度253mW·cm~(-2),并且开路电压在20min内降低,原因是还原过程阳极体积的变化导致电解质破裂。
SLABS3与SOFC组元共烧时粘接性良好。能谱分析表明,向微晶玻璃方向,与NiO/YSZ阳极共烧Zr的扩散深度10μm;与阴极共烧Mn的扩散深度60μm;与连接体共烧,Cr和Fe的扩散深度约20μm,但是微晶玻璃的成分却没有向相邻组元扩散,符合兼容性要求。制备的模拟电池用该密封材料隔离H2和O2,开路电压热循环6次仍保持在1.05V左右,表明SLABS3密封的模拟电池的气密性和稳定性良好。
由于硬密封导致电池无法拆卸,同时研究了云母和气相SiO2填充的陶瓷纤维作为压实密封材料。结果表明,采用气相SiO2填充的陶瓷纤维的泄漏率随气相SiO2填充量的增加而减小。填充的陶瓷纤维预压后在1MPa压力,10kPa气压差下泄漏率仅为0.04sccm·cm~(-1),密封性能优于云母,该泄漏率值低于文献报道水平,达到国际先进水平,并且热循环20次保持稳定,在800℃下H2还原200h质量损失速率为1.7×10~(-2)g·cm~(-2)·h~(-1),还原后不影响泄漏率。
Solid oxide fuel cell (SOFC) has the advantage of all solid component and high conversion efficiency, which is as high as 80%, so it is one of the focus study in the world. Normally the anode electrode and electrolyte were co-sintered together. To prevent the mixture of oxygen and hydrogen at high temperature, seals, which were pasted on anode electrode, were required.
Line structure of starch and ball structure of polymethyl methacrylate( PMMA) as pore-formers for SOFC anode supported layer were compared. The results demonstrated that the the porosity was 29.8%, electronic conductivity was 2000.35S·cm~(-1) for 15mass% starch as pore-formers. But the porosity was 36.4% and 59.4%, and conductivity was 1200.0 S·cm~(-1) and 1008.45 S·cm~(-1) respectively for 15mass% and 30mass% PMMA pore-formers.
Discharging curvess for the cell prepared by different pore-formers and their contents demonstrated that when the porosity is lower than 59.4%, the Discharging property increased with the porosity, but the influence of H2 flow rate on Discharging curve is not obvious when the porosity is 59.4%. Three average particle sizes higher than 1μm of NiO were studied as anode functional layer. The cell performance is the highest for the cell prepared NiO-,with the maxium powder density 121 mW·cm~(-2) ,but only 81 mW·cm~(-2) for NiO-.Scanning electron microscope (SEM) images showed that the particle size of NiO-Ⅰwas about 2μm, but 4.47μm for NiO-Ⅲ.To reduce the NiO particle size, nano NiO-Ⅳproduced by co-precipitation and commercial NiO-Ⅴwere used as SOFC anode functional layer. The maximum power density of the cell was 205.3mW·cm~(-2) and 308.2mW·cm~(-2) respectively, and the cell power density prepared from NiO-Ⅴcalcined at 700℃increased to 369.0mW·cm~(-2) .YSZ coarsened at 1200℃and milled for 12h let the cell power density increase to 390.5mW·cm~(-2).
Dimension of JC 8YSZ and TOSOH 8YSZ ,which were widely used as SOFC electrolye, were measured. The results showed that they shrinked at 1000℃. The total shrinkage of JC YSZ was 25.2%, but that of TOSOH 8YSZ was 19.0%. Particle analysis showed that the average particle size of TOSOH 8YSZ was 0.71μm, only about 2.5fold of that JC 8YSZ, which was 1.91μm. The electrochemical analynis demonstrated that the electronic donductivity of JC 8YSZ and TOSOH 8YSZ at 800℃were 0.0179S·cm~(-1) and 0.0212 S·cm~(-1) respectively. The calculated activation energies were 108.35kJ·mol~(-1) and 105.67kJ·mol~(-1) respectively. The maximum powder density of the cells made up of these two 8YSZ at 800℃were 184.08 mW·cm~(-2) for JC 8YSZ and 267.75 mW·cm~(-2) for TOSOH 8YSZ. SEM images showed that none of the electrolyte made of this two YSZ was dense, but was denser made of 80%JC YSZ and 20%TOSOH YSZ mixture. When the thickness of the electrolyte was 20μm, the open current voltage of the electrolyte was 1002mV and its power density reached 447mW·cm~(-2) while kept stable. However, when the thickness reduced to 13μm, there was only 253mW·cm~(-2) for the power density, and 923mV for the OCV, and decreased in 20min. The reason was that the voltage change during anode reduction led to YSZ electrolyte crack.
SLABS3 ceramic glass“glue”SOFC other components well. During co-calcined for 100h, Zr element diffused 10μm to glass, Mn with 60μm , Cr and Fe element about 20μm, but none element of the glass would diffuse to SOFC other components, which meet the requirement of compatibility.The OCV test remained higher than 1.05V,demonstrating that seals meet the requirement in 6 circles.
However, as the solid seals cause the problem of stack unable replacement, so compressive seals were also studied. Leakage test for alumina silica infiltrated ceramic fiber paper and mica were studied. The results demonstrated that the leakage of the infiltrated ceramic fiber paper was 0.04sccm·cm~(-1), which was lower than that of mica. This value is lower than the leakage reported. The infiltrated ceramic fiber paper were stabe in 20 thermal cycles and the weight loss at 800℃under hydrogen atmosphere was 1.7×10~(-2)g·cm~(-2)·h~(-1) for 200h, which showed no effect on sealing performance.
引文
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128 综研化学.http://www.soken-sz.com
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