固体氧化物燃料电池密封材料设计与性能优化
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摘要
固体氧化物燃料电池(Solid Oxide Fuel Cell,SOFC)是一种高效、清洁、安静和可靠的电化学发电装置,适合作为分散、移动电源或大中型电站,在电力、运输及军事方面均具有广阔的应用前景。出于未来能源战略、环境保护考虑,世界各国一直致力于SOFC发电技术的研究和开发。然而,高温密封问题一直是制约平板式SOFC发展的主要技术难点之一。本论文以中温固体氧化物燃料电池(Intermediate Temperature Solid Oxide Fuel Cell,IT-SOFC)技术为背景,研究开发能够满足平板式IT-SOFC的密封要求的压缩式密封材料。
本论文首先分析了平板式IT-SOFC密封的特殊性,针对平板式IT-SOFC密封中可能发生的界面泄漏和渗透泄漏,分别建立了一系列流体力学计算模型,对不同条件下气体的泄漏量进行了理论计算与分析。在此基础上,选择陶瓷密封材料作为研究对象,对其结构进行了设计,确定了以Al_2O_3微粉为主的原料体系和流延制备工艺。系统研究了Al_2O_3微粉种类、分散剂、粘结剂、增塑剂、真空除气工艺以及干燥制度等因素对材料流延成型制备的影响,优化了流延成型制备技术。研制了IT-SOFC密封性能测试平台,对Al_2O_3密封材料和添加Al或BaO-B_2O_3-SiO_2玻璃的Al_2O_3基复合密封材料的密封性能进行表征,系统研究了Al_2O_3粉体微观特征、外加载荷以及材料复合等因素对材料密封性能的影响。为了判断上述密封材料在IT-SOFC中的实用性,选择密封性能良好的密封材料进行了SOFC单电池测试。上述研究结果表明:
(1)具有优良化学稳定性、绝缘性和化学相容性的陶瓷材料是平板式IT-SOFC密封材料的首要选择。理论计算表明,每厘米宽度陶瓷密封材料上氢气泄漏的质量流率必须小于7.35×10~(-8) g·s~(-1),从而要求陶瓷密封材料必须能够消除界面泄漏,将原料粒度分布的D50值控制在1～2μm范围以使绝大部分漏气通道的有效尺寸小于1μm,以及尽可能减小材料的有效孔隙率和增加材料中漏气通道的迂曲度。
(2)采用优化的流延成型技术可以制备出表面平整、厚度均匀、柔韧性良好的Al_2O_3密封材料和Al_2O_3基复合密封材料。这些材料均具有较好的耐压能力,其变形能力能够满足IT-SOFC密封装配的需要。
(3)Al_2O_3密封材料和Al_2O_3基复合密封材料在较小外加载荷下表现出较好的密封性能。所有密封材料的漏气率均随着外加载荷增加而下降,随通气压力的增加而增加。不同Al_2O_3密封材料性能之间的差异主要与这些材料的微观特征有关。
(4)添加Al微粉可以改善Al_2O_3密封材料密封性能。Al在升温过程中的软化、变形以及伴随Al氧化生成Al_2O_3所产生的体积膨胀均可以减少材料中的漏气通道和降低材料的孔隙率。通过Al的反应键合,可以将数个Al_2O_3颗粒联结起来,在某种程度上也增加了漏气通道的迂曲度。
(5)BaO-B_2O_3-SiO_2玻璃微粉的加入对Al_2O_3密封材料密封性能的影响较为复杂。添加BaO-B_2O_3-SiO_2玻璃微粉必须与能够产生有利的反应胶结效应相对应的外加载荷配合才能提高Al_2O_3密封材料的密封性能。
(6)Al_2O_3密封材料的密封稳定性与材料的微结构稳定性有很大关系。部分Al_2O_3密封材料的漏气率随时间推移逐渐变大,与这些材料在某些区域出现新贯通孔有关。Al→Al_2O_3反应键合机制和BaO-B_2O_3-SiO_2玻璃的反应胶结作用均有助于密封稳定性的提高。
(7)单电池性能测试结果表明,采用优化流延成型技术制备的AS2-69、AS2-A10、AS2-A20和AS4-A20密封材料均能够满足平板式IT-SOFC的密封需要。
Solid Oxide Fuel Cell (SOFC) is a highly efficient, clean, quiet and reliable electric power generation device, which can be used as distributed or mobile power sources or the large-scale power plant, and has extensive applications in the sectors of power generation, transportation and military. For the sake of future energy strategy and environment protection, the SOFC technology has been under development in many countries for years. However, one of the most significant challenges for the planar SOFC design is to realize the effective high temperature sealing. With the Intermediate Temperature Solid Oxide Fuel Cell (IT-SOFC) in the background, novel compressive seals had been developed in the present study.
In this dissertation, firstly, the uniqueness of the sealing for the planar IT-SOFC was analyzed; a series of hydromechanical models aiming at the interface leak and the infiltration leak were established; and the gas leak rates under various conditions were calculated according to the models and the influencing factors were discussed. According to the above results, ceramic sealing materials were selected as the subject of study and the microstructure of the seal was designed; accordingly, Al_2O_3 fine powder was chosen as the baseline material for the seals prepared by the tape casting process. The effect of Al_2O_3 powders, dispersant, binder, plasticizer as well as deairing and drying procedures on the tape casting process were systematically investigated, and hence, the tape casting process was optimized accordingly. With a sealing assessment facility developed in house, the effectiveness of the seals prepared with Al_2O_3 and Al_2O_3-based composites with addition of Al or BaO-B_2O_3-SiO_2 glass fine powders were evaluated against the Al_2O_3 powder characteristics, compressive stresses and the addition of Al and BaO-B_2O_3-SiO_2 particles. In order to demonstrate the applicability to the IT-SOFC, single cell tests with the developed seals were conducted. The major results obtained are described as follow:
(1) Materials with high chemical stability, insulativity and chemical compatibility in the IT-SOFC environment are preferred the sealing application. The theoretic calculations indicated that a hydrogen leak rate of the ceramic seals per centimeter must be less than 7.35×10~(-8) g·s~(-1).Therefore, the interface leak should be eliminated, the D50 value of the ceramic raw materials should be in range of 1~2μm to keep the effective leak path less than 1μm, and the effective porosity of the seals should decrease and the tortuosity of leak path should increase as possible.
(2) The optimized tape casting process is a correct choice for fabricating the Al_2O_3 and Al_2O_3-based composite seals with smooth surfaces, uniform thickness and excellent flexibility. These seals all have acceptable compressive strength, and their deformability is adequate to satisfy the need for IT-SOFC sealing assembly.
(3) Satisfactory sealing effect is offered with the Al_2O_3 and Al_2O_3-based composite seals under slight applied loads. The leak rate of the seals decreases with increasing the compressive stress and decreasing the gauge pressure. The difference in sealing effectiveness between seals prepared with various Al_2O_3 powders is mainly correlated to their powder characteristics.
(4) The addition of Al fine powders can significantly improve the sealing properties of the Al_2O_3 seals. The softening and deformation of Al particles upon heating and the volume expansion (28%) associated with Al oxidation can reduce the leak path and porosity of the seals. The reaction bonding generated from Al oxidation is expected to cluster individual Al_2O_3 particles, effectively increasing the tortuosity the leak paths.
(5) The influence of the BaO-B_2O_3-SiO_2 glass fine powder addition on the Al_2O_3 seals is complex. The sealing effectiveness can be enhanced under compressive stresses that are causing the advantageous reaction cementation.
(6) The sealing stability of the Al_2O_3 seals is closely related to the stability of their microstructures. The leak rate increases with time in some Al_2O_3 seals can be attributed to the occurrence of new leak paths due to localized microstructure instability. The reaction bonding from the Al oxidation and reaction cementation from the BaO-B_2O_3-SiO_2O glass can improve the stability of the seals.
(7) Single cell tests with tape cast AS2-69, AS2-A10, AS2-A20 and AS4-A20 seals have confirmed the applicability of the developed seals to planar IT-SOFCs.
本论文首先分析了平板式IT-SOFC密封的特殊性,针对平板式IT-SOFC密封中可能发生的界面泄漏和渗透泄漏,分别建立了一系列流体力学计算模型,对不同条件下气体的泄漏量进行了理论计算与分析。在此基础上,选择陶瓷密封材料作为研究对象,对其结构进行了设计,确定了以Al_2O_3微粉为主的原料体系和流延制备工艺。系统研究了Al_2O_3微粉种类、分散剂、粘结剂、增塑剂、真空除气工艺以及干燥制度等因素对材料流延成型制备的影响,优化了流延成型制备技术。研制了IT-SOFC密封性能测试平台,对Al_2O_3密封材料和添加Al或BaO-B_2O_3-SiO_2玻璃的Al_2O_3基复合密封材料的密封性能进行表征,系统研究了Al_2O_3粉体微观特征、外加载荷以及材料复合等因素对材料密封性能的影响。为了判断上述密封材料在IT-SOFC中的实用性,选择密封性能良好的密封材料进行了SOFC单电池测试。上述研究结果表明:
(1)具有优良化学稳定性、绝缘性和化学相容性的陶瓷材料是平板式IT-SOFC密封材料的首要选择。理论计算表明,每厘米宽度陶瓷密封材料上氢气泄漏的质量流率必须小于7.35×10~(-8) g·s~(-1),从而要求陶瓷密封材料必须能够消除界面泄漏,将原料粒度分布的D50值控制在1～2μm范围以使绝大部分漏气通道的有效尺寸小于1μm,以及尽可能减小材料的有效孔隙率和增加材料中漏气通道的迂曲度。
(2)采用优化的流延成型技术可以制备出表面平整、厚度均匀、柔韧性良好的Al_2O_3密封材料和Al_2O_3基复合密封材料。这些材料均具有较好的耐压能力,其变形能力能够满足IT-SOFC密封装配的需要。
(3)Al_2O_3密封材料和Al_2O_3基复合密封材料在较小外加载荷下表现出较好的密封性能。所有密封材料的漏气率均随着外加载荷增加而下降,随通气压力的增加而增加。不同Al_2O_3密封材料性能之间的差异主要与这些材料的微观特征有关。
(4)添加Al微粉可以改善Al_2O_3密封材料密封性能。Al在升温过程中的软化、变形以及伴随Al氧化生成Al_2O_3所产生的体积膨胀均可以减少材料中的漏气通道和降低材料的孔隙率。通过Al的反应键合,可以将数个Al_2O_3颗粒联结起来,在某种程度上也增加了漏气通道的迂曲度。
(5)BaO-B_2O_3-SiO_2玻璃微粉的加入对Al_2O_3密封材料密封性能的影响较为复杂。添加BaO-B_2O_3-SiO_2玻璃微粉必须与能够产生有利的反应胶结效应相对应的外加载荷配合才能提高Al_2O_3密封材料的密封性能。
(6)Al_2O_3密封材料的密封稳定性与材料的微结构稳定性有很大关系。部分Al_2O_3密封材料的漏气率随时间推移逐渐变大,与这些材料在某些区域出现新贯通孔有关。Al→Al_2O_3反应键合机制和BaO-B_2O_3-SiO_2玻璃的反应胶结作用均有助于密封稳定性的提高。
(7)单电池性能测试结果表明,采用优化流延成型技术制备的AS2-69、AS2-A10、AS2-A20和AS4-A20密封材料均能够满足平板式IT-SOFC的密封需要。
Solid Oxide Fuel Cell (SOFC) is a highly efficient, clean, quiet and reliable electric power generation device, which can be used as distributed or mobile power sources or the large-scale power plant, and has extensive applications in the sectors of power generation, transportation and military. For the sake of future energy strategy and environment protection, the SOFC technology has been under development in many countries for years. However, one of the most significant challenges for the planar SOFC design is to realize the effective high temperature sealing. With the Intermediate Temperature Solid Oxide Fuel Cell (IT-SOFC) in the background, novel compressive seals had been developed in the present study.
In this dissertation, firstly, the uniqueness of the sealing for the planar IT-SOFC was analyzed; a series of hydromechanical models aiming at the interface leak and the infiltration leak were established; and the gas leak rates under various conditions were calculated according to the models and the influencing factors were discussed. According to the above results, ceramic sealing materials were selected as the subject of study and the microstructure of the seal was designed; accordingly, Al_2O_3 fine powder was chosen as the baseline material for the seals prepared by the tape casting process. The effect of Al_2O_3 powders, dispersant, binder, plasticizer as well as deairing and drying procedures on the tape casting process were systematically investigated, and hence, the tape casting process was optimized accordingly. With a sealing assessment facility developed in house, the effectiveness of the seals prepared with Al_2O_3 and Al_2O_3-based composites with addition of Al or BaO-B_2O_3-SiO_2 glass fine powders were evaluated against the Al_2O_3 powder characteristics, compressive stresses and the addition of Al and BaO-B_2O_3-SiO_2 particles. In order to demonstrate the applicability to the IT-SOFC, single cell tests with the developed seals were conducted. The major results obtained are described as follow:
(1) Materials with high chemical stability, insulativity and chemical compatibility in the IT-SOFC environment are preferred the sealing application. The theoretic calculations indicated that a hydrogen leak rate of the ceramic seals per centimeter must be less than 7.35×10~(-8) g·s~(-1).Therefore, the interface leak should be eliminated, the D50 value of the ceramic raw materials should be in range of 1~2μm to keep the effective leak path less than 1μm, and the effective porosity of the seals should decrease and the tortuosity of leak path should increase as possible.
(2) The optimized tape casting process is a correct choice for fabricating the Al_2O_3 and Al_2O_3-based composite seals with smooth surfaces, uniform thickness and excellent flexibility. These seals all have acceptable compressive strength, and their deformability is adequate to satisfy the need for IT-SOFC sealing assembly.
(3) Satisfactory sealing effect is offered with the Al_2O_3 and Al_2O_3-based composite seals under slight applied loads. The leak rate of the seals decreases with increasing the compressive stress and decreasing the gauge pressure. The difference in sealing effectiveness between seals prepared with various Al_2O_3 powders is mainly correlated to their powder characteristics.
(4) The addition of Al fine powders can significantly improve the sealing properties of the Al_2O_3 seals. The softening and deformation of Al particles upon heating and the volume expansion (28%) associated with Al oxidation can reduce the leak path and porosity of the seals. The reaction bonding generated from Al oxidation is expected to cluster individual Al_2O_3 particles, effectively increasing the tortuosity the leak paths.
(5) The influence of the BaO-B_2O_3-SiO_2 glass fine powder addition on the Al_2O_3 seals is complex. The sealing effectiveness can be enhanced under compressive stresses that are causing the advantageous reaction cementation.
(6) The sealing stability of the Al_2O_3 seals is closely related to the stability of their microstructures. The leak rate increases with time in some Al_2O_3 seals can be attributed to the occurrence of new leak paths due to localized microstructure instability. The reaction bonding from the Al oxidation and reaction cementation from the BaO-B_2O_3-SiO_2O glass can improve the stability of the seals.
(7) Single cell tests with tape cast AS2-69, AS2-A10, AS2-A20 and AS4-A20 seals have confirmed the applicability of the developed seals to planar IT-SOFCs.
引文
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