中低温固体氧化物燃料电池双层电解质的脉冲激光制备及电化学研究
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摘要
为了实现固体氧化物燃料电池(SOFCs)商业化发展,最关键的因素是降低SOFCs工作温度至中低温化,而发展高电导率SOFCs电解质材料和电解质薄膜化是解决SOFCs中低温化带来的欧姆损失问题的关键。目前研究较多的SOFCs电解质材料有掺杂的CeO2, LaGaO3及稳定的ZrO2基氧离子导体和掺杂的BaCeO3, BaZrO3基质子导体材料。本论文围绕上述几种电解质材料,在电解质结构设计、电解质薄膜的制备技术以及电化学性能优化方面进行研究。
第一章主要介绍氧离子导体基SOFCs和质子导体基SOFCs的研究背景、发展状况和工作原理,总结了SOFCs电解质材料以及各自存在的问题,阐述了双层电解质结构的概念,并讨论将这种结构与SOFCs电解质材料相结合并应用的可能性。同时也分析了几种常用的电解质薄膜制备技术。
第二章采用脉冲激光沉积法(PLD)成功的在阳极支撑的SDC电解质层表面制备出致密的8mol%Y2O3稳定的ZrO2(YSZ)电子阻隔层和Ce0.8Sm0.2O2-δ(SDC)缓冲层。实验结果表明由于PLD镀膜时衬底温度较低,从而可以避免传统化学法在高温烧结下容易引起CeO2和ZrO2层之间的界面反应。当YSZ层引入电解质结构中,相应的燃料电池开路电压(OCV)得到明显提高,表明PLD制备的YSZ层十分致密,能够有效阻隔Ce4+还原所产生的电子电导。通过在SDC/YSZ双层电解质表面沉积一层SDC缓冲层,不仅避免Smo.5Sro.5Co03-6(SSC)阴极和YSZ之间的反应和热膨胀不匹配问题,同时也降低了极化损失,获得较好的电池性能。上述结论表明PLD技术作为一种能在低温下沉积高质量薄膜的镀膜手段,可以广泛应用于SOFCs电解质薄膜的制备与研究。
第三章通过对阳极衬底的优化,讨论了衬底表面形貌和结构对PLD制备的薄膜质量的影响。实验结果表明若在未优化的阳极上沉积薄膜,由于薄膜厚度相比于孔洞尺寸较小,造成难以完全覆盖阳极缺陷,在经过电池测试还原后阳极/电解质薄膜界面会出现裂纹,影响电池整体结构和电化学性能。经过功能层优化修复了表面尺寸较大的孔洞,在这种衬底上所制备的薄膜平整且未发现裂纹。此外,我们还比较了在两种不同阳极衬底上利用PLD技术制备YSZ/SDC双层电解质薄膜所对应的电池性能。在未优化衬底上制备的单电池性能衰减很快,而在优化的阳极衬底上制备的单电池获得了相当高的最大功率密度,750℃达到1.19Wcm-2,并且保持很好的长期稳定性,开路电压在750℃达到0.959V,远高于SDC单电解质电池性能,结果表明阳极优化对电池的性能和结构稳定性都有很大的帮助。
第四章探讨了PLD沉积条件对(LSGM)薄膜质量的影响。基于LSGM具有很高的离子电导率,我们设计采用PLD技术在SDC半电池上制备LSGM电子阻隔层,探索沉积过程中氧分压大小以及后续退火温度对LSGM薄膜形貌、组分、粗糙度和相结构性质的影响。综合LSGM薄膜的沉积速度,质量以及化学计量比考虑,得出PLD制备过程中的最佳氧分压值。为了解决LSGM薄膜相结构的问题,我们研究不同退火温度对LSGM成相的影响,发现退火温度越高,LSGM结晶性越好,但高温容易造成Ga流失。最终我们将沉积的LSGM薄膜与阴极采取一步煅烧,既简化工艺流程又保证薄膜结晶度,也防止Ga挥发。此外,我们也研究了不同退火处理对应的SDC/LSGM双层电解质燃料电池的电化学性能,结果表明将LSGM退火与阴极煅烧在一个过程中完成,这样得到的电池性能最佳。SDC/LSGM双层电解质电池结构既起到了阻隔Ce4+产生的电子电导,同时也保护LSGM不与Ni基阳极反应,维持了良好的结构稳定性。
第五章通过PLD技术在阳极支撑的BaCeo.8Yo.203-δ(BCY)电解质层表面制备BaZr0.8Yo.203-δ(BZY)薄膜,讨论不同厚度的BZY薄膜对BCY的化学稳定性和相应电化学性能的影响。实验结果表明当BZY厚度达到一定大小,对应的BCY/BZY双层电解质膜才能在CO2气氛中获得较好的化学稳定性。然而由于BZY厚度增加造成欧姆电阻增加,此外阴极与BZY匹配性较差,极化损失严重,从而相应的单电池最大功率密度随着BZY厚度增加而降低。通过实验结果得出,具有一定厚度的BZY对应的BCY/BZY双层电解质电池显示出良好的化学稳定性,并具有可观的电导率和电化学性能。
第六章基于BaZro.7Pro.1Yo.203.6(BZPY)具有比BZY更高的电导率,实验采用PLD技术在BCY电解质表面制备BZPY薄膜,研究BCY/BZPY双层电解质膜的化学稳定性和电化学性能。实验结果表明BCY/BZPY双层电解质结构不仅具有很好的化学稳定性,而且在膜电导率及电池性能方面都比BCY/BZY性能有所提高,在700℃下单电池最大功率密度为250mW cm-2,双层膜电导率为6.02×10-3S cm-1,与传统稀土元素掺杂的BaCeO3基电解质性能也是可比的,表明BZPY层的引入不仅能有效的保护BCY结构不受C02影响,维持化学稳定性,同时也能保证较好的电池性能,作为质子导体基SOFCs电解质材料具有可观的发展前途。
第七章对本论文的工作进行总结,并对双层电解质SOFCs以后的研究工作进行展望。
The key factor to achieve the commercialization development of solid oxide fuel cells (SOFCs) is to decrease the operating temperarute of SOFCs down to intermediate-low range. To solve the ohmic loss caused by decreasing operating temperature, it is urgent to find SOFCs electrolytes with high ionic conductivity and reducing electrolyte thickness. Ionic-conducting materials such as doped CeO2, LaGaO3and stabilized Z1O2, and proton-conducting materials such as doped BaCeO3and BaZrO3are well developed SOFCs electrolyte materials. The thesis is focused on those electrolyte materials and discussed the electrolyte structure, fim fabrication techniques and electrochemical performance of SOFCs.
Chapter1mainly described the research background, development status and working principles of SOFCs, including ionic-conducting and proton-conducting SOFCs, summarized SOFCs electrolyte materials and their problems, introducesd the concept of bilayer electrolytes and discussed the possibilities of conbine the structure with SOFCs electrolytes. Besides, common fabrication techniques of electrolyte membrane were included.
In Chapter2, pulse laser deposition (PLD) technique was succesfully introduced in fabricating dense8mo1%Y2O3stabilized ZrO2(YSZ) electronic-blocking layer and Ceo.8Smo.202-5(SDC)buffer layer. As the deposition temperature is low, thus inerfacial reaction between the doped ceria and stabilized zirconia can avoided. After incorporating YSZ film as electrolyte layer, the open circuit voltage (OCV) of fuel cell improved significantly indicating the YSZ film deposited by PLD technique is dense enough to block the eletronic conduction caused by Ce4+reduction. With SDC buffer layer deposited on the bilayer electrolytes, thermal mismatch and chemical reaction between Smo.5Sro.5CoO3-δ (SSC) cathode and YSZ layer can be avoided, also the polarization loss was reduced and cell performance was improved. The results indicate that as an excellent film fabrication technique, PLD can be used in the researchment of SOFCs electrolyte films.
Chapter3discussed the influence of substrate morphology on the quality of PLD deposited fims. The research results show that when electrolytes were directly deposited on anode substrate, the films could not cover anode pores due to the smaller size of film thickness than pores, and the interface between electrolyte and anode appeared cracks after reducing in H2, thus influenced the whole cell structure and electrochemical performance. With functional layer optimized anode pores, deposited YSZ/SDC bilayer electrolyte films were uniform without any cracks. The corresponding fuel cell has an excellent electrical performance, the maximum power density of1.19W cm-2and open circuit voltage (OCV) of0.959V was achieved at750℃which shows an improvement in SDC single electrolyte cell, indicating anode optimization has a great asistant on cell performance and structure stability.
In Chapter4, the effect of deposition parameters on the quality of Lao.9Sro.1Gao.gMgo.203-δ (LSGM) thin film in PLD process were reserached. As LSGM has high ion conductivity and was incorporated as electronic-blocking layer onto SDC electrolyte. The oxygen pressure and post-annealing temperatures were investigated their influence on surface morphology, element component, roughness and phase structure. In terms of the quality, deposition rate and composition of the LSGM film deposited by PLD technique, the proper oxygen pressure seems to be0.67Pa. In order to improve the crystallinity of the deposited LSGM films, the suitable method is the one-step process which means keeping the cathode firing and the post-annealing procedure in the same process. The experiment results indicate that SDC/LSGM bilayer electrolyte structure has good mechanical stability, which not only blocks the electronic conduction, bue also prohibits the reaction between LSGM and Ni-base anode.
In Chapter5, BaZro.8Yo.203-δ (BZY) films were incorporated onto BaCe0.8Yo.203-δ (BCY) electrolytes with PLD technique and the effect of BZY films thicknesses on chemical stability and electrochemical performance was investigated. Only when BZY film achieves to a certain thickness, BZY layer can protect BCY in CO2atmosphere. With increasing thickness of BZY layer, the ohmic resistance increases, besides the poor matching between BZY layer and cathode caused bad polarization loss, thus the corresponding fuel cell has a lower electrochemical performance. The research results indicate that BCY/BZY bilayer electrolyte fuel cell, with cetain thickness of BZY layer, has good chemical stability and considerable electrochemical performance.
In Chapter6, based on the better conductivity of BaZr0.7Pr0.1Y0.2O3-δ (BZPY) than BZY, BZPY thin film was fabricated on BCY electrolyte with PLD technique. BCY/BZPY bilayer electrolyte structure shows an excellent chemical stability. Besides, the membrane conductivity and fuel cell performance improves a lot in BCY/BZPY bilayer electrolyte fuel cell, the maximum power density at700℃is250 mW cm-2, the membrane conductivity at700℃is6.02×10"3S cm-1, which are both comparable with tranditional rare earth doped BaCeO3electrolyte cell. The results indicate that BCY/BZPY bilayer electrolyte structure has good chemical stability and electrochemical performance and has good future as proton-condictiong SOFCs electrolytes.
In Chaper7, the works presented in the thesis are concluded and future research on bilayer electrolyte SOFCs is proposed
第一章主要介绍氧离子导体基SOFCs和质子导体基SOFCs的研究背景、发展状况和工作原理,总结了SOFCs电解质材料以及各自存在的问题,阐述了双层电解质结构的概念,并讨论将这种结构与SOFCs电解质材料相结合并应用的可能性。同时也分析了几种常用的电解质薄膜制备技术。
第二章采用脉冲激光沉积法(PLD)成功的在阳极支撑的SDC电解质层表面制备出致密的8mol%Y2O3稳定的ZrO2(YSZ)电子阻隔层和Ce0.8Sm0.2O2-δ(SDC)缓冲层。实验结果表明由于PLD镀膜时衬底温度较低,从而可以避免传统化学法在高温烧结下容易引起CeO2和ZrO2层之间的界面反应。当YSZ层引入电解质结构中,相应的燃料电池开路电压(OCV)得到明显提高,表明PLD制备的YSZ层十分致密,能够有效阻隔Ce4+还原所产生的电子电导。通过在SDC/YSZ双层电解质表面沉积一层SDC缓冲层,不仅避免Smo.5Sro.5Co03-6(SSC)阴极和YSZ之间的反应和热膨胀不匹配问题,同时也降低了极化损失,获得较好的电池性能。上述结论表明PLD技术作为一种能在低温下沉积高质量薄膜的镀膜手段,可以广泛应用于SOFCs电解质薄膜的制备与研究。
第三章通过对阳极衬底的优化,讨论了衬底表面形貌和结构对PLD制备的薄膜质量的影响。实验结果表明若在未优化的阳极上沉积薄膜,由于薄膜厚度相比于孔洞尺寸较小,造成难以完全覆盖阳极缺陷,在经过电池测试还原后阳极/电解质薄膜界面会出现裂纹,影响电池整体结构和电化学性能。经过功能层优化修复了表面尺寸较大的孔洞,在这种衬底上所制备的薄膜平整且未发现裂纹。此外,我们还比较了在两种不同阳极衬底上利用PLD技术制备YSZ/SDC双层电解质薄膜所对应的电池性能。在未优化衬底上制备的单电池性能衰减很快,而在优化的阳极衬底上制备的单电池获得了相当高的最大功率密度,750℃达到1.19Wcm-2,并且保持很好的长期稳定性,开路电压在750℃达到0.959V,远高于SDC单电解质电池性能,结果表明阳极优化对电池的性能和结构稳定性都有很大的帮助。
第四章探讨了PLD沉积条件对(LSGM)薄膜质量的影响。基于LSGM具有很高的离子电导率,我们设计采用PLD技术在SDC半电池上制备LSGM电子阻隔层,探索沉积过程中氧分压大小以及后续退火温度对LSGM薄膜形貌、组分、粗糙度和相结构性质的影响。综合LSGM薄膜的沉积速度,质量以及化学计量比考虑,得出PLD制备过程中的最佳氧分压值。为了解决LSGM薄膜相结构的问题,我们研究不同退火温度对LSGM成相的影响,发现退火温度越高,LSGM结晶性越好,但高温容易造成Ga流失。最终我们将沉积的LSGM薄膜与阴极采取一步煅烧,既简化工艺流程又保证薄膜结晶度,也防止Ga挥发。此外,我们也研究了不同退火处理对应的SDC/LSGM双层电解质燃料电池的电化学性能,结果表明将LSGM退火与阴极煅烧在一个过程中完成,这样得到的电池性能最佳。SDC/LSGM双层电解质电池结构既起到了阻隔Ce4+产生的电子电导,同时也保护LSGM不与Ni基阳极反应,维持了良好的结构稳定性。
第五章通过PLD技术在阳极支撑的BaCeo.8Yo.203-δ(BCY)电解质层表面制备BaZr0.8Yo.203-δ(BZY)薄膜,讨论不同厚度的BZY薄膜对BCY的化学稳定性和相应电化学性能的影响。实验结果表明当BZY厚度达到一定大小,对应的BCY/BZY双层电解质膜才能在CO2气氛中获得较好的化学稳定性。然而由于BZY厚度增加造成欧姆电阻增加,此外阴极与BZY匹配性较差,极化损失严重,从而相应的单电池最大功率密度随着BZY厚度增加而降低。通过实验结果得出,具有一定厚度的BZY对应的BCY/BZY双层电解质电池显示出良好的化学稳定性,并具有可观的电导率和电化学性能。
第六章基于BaZro.7Pro.1Yo.203.6(BZPY)具有比BZY更高的电导率,实验采用PLD技术在BCY电解质表面制备BZPY薄膜,研究BCY/BZPY双层电解质膜的化学稳定性和电化学性能。实验结果表明BCY/BZPY双层电解质结构不仅具有很好的化学稳定性,而且在膜电导率及电池性能方面都比BCY/BZY性能有所提高,在700℃下单电池最大功率密度为250mW cm-2,双层膜电导率为6.02×10-3S cm-1,与传统稀土元素掺杂的BaCeO3基电解质性能也是可比的,表明BZPY层的引入不仅能有效的保护BCY结构不受C02影响,维持化学稳定性,同时也能保证较好的电池性能,作为质子导体基SOFCs电解质材料具有可观的发展前途。
第七章对本论文的工作进行总结,并对双层电解质SOFCs以后的研究工作进行展望。
The key factor to achieve the commercialization development of solid oxide fuel cells (SOFCs) is to decrease the operating temperarute of SOFCs down to intermediate-low range. To solve the ohmic loss caused by decreasing operating temperature, it is urgent to find SOFCs electrolytes with high ionic conductivity and reducing electrolyte thickness. Ionic-conducting materials such as doped CeO2, LaGaO3and stabilized Z1O2, and proton-conducting materials such as doped BaCeO3and BaZrO3are well developed SOFCs electrolyte materials. The thesis is focused on those electrolyte materials and discussed the electrolyte structure, fim fabrication techniques and electrochemical performance of SOFCs.
Chapter1mainly described the research background, development status and working principles of SOFCs, including ionic-conducting and proton-conducting SOFCs, summarized SOFCs electrolyte materials and their problems, introducesd the concept of bilayer electrolytes and discussed the possibilities of conbine the structure with SOFCs electrolytes. Besides, common fabrication techniques of electrolyte membrane were included.
In Chapter2, pulse laser deposition (PLD) technique was succesfully introduced in fabricating dense8mo1%Y2O3stabilized ZrO2(YSZ) electronic-blocking layer and Ceo.8Smo.202-5(SDC)buffer layer. As the deposition temperature is low, thus inerfacial reaction between the doped ceria and stabilized zirconia can avoided. After incorporating YSZ film as electrolyte layer, the open circuit voltage (OCV) of fuel cell improved significantly indicating the YSZ film deposited by PLD technique is dense enough to block the eletronic conduction caused by Ce4+reduction. With SDC buffer layer deposited on the bilayer electrolytes, thermal mismatch and chemical reaction between Smo.5Sro.5CoO3-δ (SSC) cathode and YSZ layer can be avoided, also the polarization loss was reduced and cell performance was improved. The results indicate that as an excellent film fabrication technique, PLD can be used in the researchment of SOFCs electrolyte films.
Chapter3discussed the influence of substrate morphology on the quality of PLD deposited fims. The research results show that when electrolytes were directly deposited on anode substrate, the films could not cover anode pores due to the smaller size of film thickness than pores, and the interface between electrolyte and anode appeared cracks after reducing in H2, thus influenced the whole cell structure and electrochemical performance. With functional layer optimized anode pores, deposited YSZ/SDC bilayer electrolyte films were uniform without any cracks. The corresponding fuel cell has an excellent electrical performance, the maximum power density of1.19W cm-2and open circuit voltage (OCV) of0.959V was achieved at750℃which shows an improvement in SDC single electrolyte cell, indicating anode optimization has a great asistant on cell performance and structure stability.
In Chapter4, the effect of deposition parameters on the quality of Lao.9Sro.1Gao.gMgo.203-δ (LSGM) thin film in PLD process were reserached. As LSGM has high ion conductivity and was incorporated as electronic-blocking layer onto SDC electrolyte. The oxygen pressure and post-annealing temperatures were investigated their influence on surface morphology, element component, roughness and phase structure. In terms of the quality, deposition rate and composition of the LSGM film deposited by PLD technique, the proper oxygen pressure seems to be0.67Pa. In order to improve the crystallinity of the deposited LSGM films, the suitable method is the one-step process which means keeping the cathode firing and the post-annealing procedure in the same process. The experiment results indicate that SDC/LSGM bilayer electrolyte structure has good mechanical stability, which not only blocks the electronic conduction, bue also prohibits the reaction between LSGM and Ni-base anode.
In Chapter5, BaZro.8Yo.203-δ (BZY) films were incorporated onto BaCe0.8Yo.203-δ (BCY) electrolytes with PLD technique and the effect of BZY films thicknesses on chemical stability and electrochemical performance was investigated. Only when BZY film achieves to a certain thickness, BZY layer can protect BCY in CO2atmosphere. With increasing thickness of BZY layer, the ohmic resistance increases, besides the poor matching between BZY layer and cathode caused bad polarization loss, thus the corresponding fuel cell has a lower electrochemical performance. The research results indicate that BCY/BZY bilayer electrolyte fuel cell, with cetain thickness of BZY layer, has good chemical stability and considerable electrochemical performance.
In Chapter6, based on the better conductivity of BaZr0.7Pr0.1Y0.2O3-δ (BZPY) than BZY, BZPY thin film was fabricated on BCY electrolyte with PLD technique. BCY/BZPY bilayer electrolyte structure shows an excellent chemical stability. Besides, the membrane conductivity and fuel cell performance improves a lot in BCY/BZPY bilayer electrolyte fuel cell, the maximum power density at700℃is250 mW cm-2, the membrane conductivity at700℃is6.02×10"3S cm-1, which are both comparable with tranditional rare earth doped BaCeO3electrolyte cell. The results indicate that BCY/BZPY bilayer electrolyte structure has good chemical stability and electrochemical performance and has good future as proton-condictiong SOFCs electrolytes.
In Chaper7, the works presented in the thesis are concluded and future research on bilayer electrolyte SOFCs is proposed
引文
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[11]Lin B, Hu M, Ma J, Jiang Y, Tao S, Meng G. Stable, easily sintered BaCe0.5Zr0.3Y0.16Zn0.04O3-delta electrolyte-based protonic ceramic membrane fuel cells with Ba0.5Sr0.5Zn0.2Fe0.803-delta perovskite cathode. Journal of Power Sources. 2008;183:479-84.
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[13]Zhao F, Virkar AV. Dependence of polarization in anode-supported solid oxide fuel cells on various cell parameters. Journal of Power Sources.2005;141:79-95.
[14]Xia CR, Rauch W, Wellborn W, Liu ML. Functionally graded cathodes for honeycomb solid oxide fuel cells. Electrochemical and Solid State Letters.2002;5:A217-A20.
[15]Sun W, Zhu Z, Shi Z, Liu W. Chemically stable and easily sintered high-temperature proton conductor BaZr0.8In0.203-delta for solid oxide fuel cells. Journal of Power Sources. 2013;229:95-101.
[16]Wang Y, Wang H, Liu T, Chen F, Xia C. Improving the chemical stability of BaCe0.8Sm0.203-delta electrolyte by Cl doping for proton-conducting solid oxide fuel cell. Electrochemistry Communications.2013;28:87-90.
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