中温固体氧化物燃料电池硅酸镧电解质合成及性能研究
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摘要
固体氧化物燃料电池(Solid oxide fuel cell,SOFC)属于第三代燃料电池能源系统,其高能量转换效率、洁净无污染、安全方便、全固态结构和对多种燃料气体的广泛适应性等,使其应用于各个领域。高温固体氧化物燃料电池作为燃料重整和转换以及电化学反应过程等在内的无机膜反应器,把化学能直接转化为电能的效率主要决定于SOFC的核心部件-固体电解质。采用传统的ZrO_2基电解质,必须在高温下操作才能得到较高的电能转换效率,连接密封材料必须使用铂等稀贵金属,导致过高应用成本。因此,近年来研究和开发适用于中温SOFC(Intermediatetemperature solid oxide fuel cell,IT-SOFC)的新型电解质材料已成为SOFC领域的研究热点之一,其中具有低活化能和高氧离子电导率的磷灰石型硅酸镧系氧化物受到了人们的广泛关注。选择La_(10)(SiO_4)_6O_3作为应用研究的原因在于高的氧离子导电性能,低的激活能和在中温范围内(500-800℃)的良好的化学稳定性。1995年,Nakayama等人首次报道了氧磷灰石结构电解质陶瓷;2001年,Tao研究小组通过溶胶-凝胶方法在降低了200℃反应温度的条件下,成功的合成了硅酸镧粉体。随后掺杂体系的报道呈上升趋势,也得到了许多实验和理论方面的研究结果,但在有关氧离子导电机制与掺杂的物理本质的认识上还存在着很大的分歧与异议。
本论文致力于采用固相反应法合成电解质陶瓷粉体,并用等离子喷涂手段制各氧磷灰石结构硅酸镧陶瓷薄膜涂层,作为新型中温固体氧化物燃料电池电解质。利用X射线衍射技术(XRD)、差热分析(DTA)、热失重分析(TGA)、扫描电子显微镜(SEM)配备的能量弥散X射线探测器(EDX)以及电化学阻抗谱(EIS)等技术详细研究前驱体的热反应过程、合成粉体的结晶相转变过程、形貌以及电化学催化性能和电导率,通过分析比较不同工作参数获得的不同系列样品的实验结果,以期掌握影响中温反应动力学与稳定性的因素,在关键材料和复杂反应机理的研究上取得突破,为我国中温同体氧化物燃料电池技术的发展提供科学依据。
我们详细的了解和深入地调研了SOFC电解质材料及其制备工艺的研究现状(第1章)。基于对大量SOFC文献的调查研究及分析,结合我们的实际情况,形成对IT-SOFC电解质的开发研究。
我们有的放矢的选择原材料和制备工艺,并且采用适宜的测试手段,对粉体合成和工艺制备过程进行有效的跟踪监测(第2章)。
我们建议使用固相反应法合成La_(10)(SiO_4)_6O_3陶瓷粉体(第3章)。这条路线合成的优点是使结晶的复合氧化物在高温的烧结过程中有充足的反应过程和时间。事实上,固相反应法不太繁琐的操作过程和不太昂贵的试剂,使得这条路线对工业应用非常有吸引力。
我们将使用等离子喷涂手段制备陶瓷薄膜涂层(第4章)。选择这一技术是基于易于实施和规模化工业化生产的优势,同时,采用等离子喷涂制备电解质可显著降低SOFCs制造成本。
最后,这些电解质涂层的重点在于其电化学特性,通过其阻抗谱的测试,以评估其导电性,活化能及在工作温度下的稳定性(第5章)。为其在今后的工业化生产中,提供充足的基础数据支持。
In the field of electrical power generation, the development of solid oxide fuel cells (SOFCs) is limited because of their high operating temperatures. Two solutions are generally considered to decrease the temperature: reducing the thickness of the conventional yttria-stabilised zirconia (YSZ) electrolyte and / or using the new materials. The second option seems the most exploitable because novel apatite-type silicates are attracting considerable interest as a new family of oxide-ion conductors with potential use in intermediate temperature between 500 and 800℃. Among the many silicate ceramics that could be used for this application, lanthanum silicates are very promising candidates at the moment.
The objective of this thesis is the synthesis and characterization of apatite-type lanthanum silicate (ATLS) as a novel electrolyte dedicated to SOFC at intermediate temperature (IT-SOFC).
In a first step, this work is to synthesize La_(10)(SiO_4)_6O_3 powders via a solid-state reaction. Particular emphasis is placed on optimizing executive protocols. The control of synthesis parameters (nature reagents, co-grinding, sintering temperatures and residence times, etc.) can get the apatite phase in a sintering temperature between 1350℃and 1650℃. The calcined powders were used to prepare density coatings greater than 90%.
La_(10)(SiO_4))_6O_3 coatings were thermally deposited by conventional atmospheric plasma spraying (APS). The influence of projection parameters on the microstructure of coatings has been studied. The effects of porosity on the electrical properties were also discussed.
Improving the ionic conductivity is based on controlling the properties of developed coatings. For example, several sets of samples to be controlled stoichiometry have been synthesized and characterized. This study has enabled us to establish a correlation between the microstructure and conduction properties of the ceramics.
本论文致力于采用固相反应法合成电解质陶瓷粉体,并用等离子喷涂手段制各氧磷灰石结构硅酸镧陶瓷薄膜涂层,作为新型中温固体氧化物燃料电池电解质。利用X射线衍射技术(XRD)、差热分析(DTA)、热失重分析(TGA)、扫描电子显微镜(SEM)配备的能量弥散X射线探测器(EDX)以及电化学阻抗谱(EIS)等技术详细研究前驱体的热反应过程、合成粉体的结晶相转变过程、形貌以及电化学催化性能和电导率,通过分析比较不同工作参数获得的不同系列样品的实验结果,以期掌握影响中温反应动力学与稳定性的因素,在关键材料和复杂反应机理的研究上取得突破,为我国中温同体氧化物燃料电池技术的发展提供科学依据。
我们详细的了解和深入地调研了SOFC电解质材料及其制备工艺的研究现状(第1章)。基于对大量SOFC文献的调查研究及分析,结合我们的实际情况,形成对IT-SOFC电解质的开发研究。
我们有的放矢的选择原材料和制备工艺,并且采用适宜的测试手段,对粉体合成和工艺制备过程进行有效的跟踪监测(第2章)。
我们建议使用固相反应法合成La_(10)(SiO_4)_6O_3陶瓷粉体(第3章)。这条路线合成的优点是使结晶的复合氧化物在高温的烧结过程中有充足的反应过程和时间。事实上,固相反应法不太繁琐的操作过程和不太昂贵的试剂,使得这条路线对工业应用非常有吸引力。
我们将使用等离子喷涂手段制备陶瓷薄膜涂层(第4章)。选择这一技术是基于易于实施和规模化工业化生产的优势,同时,采用等离子喷涂制备电解质可显著降低SOFCs制造成本。
最后,这些电解质涂层的重点在于其电化学特性,通过其阻抗谱的测试,以评估其导电性,活化能及在工作温度下的稳定性(第5章)。为其在今后的工业化生产中,提供充足的基础数据支持。
In the field of electrical power generation, the development of solid oxide fuel cells (SOFCs) is limited because of their high operating temperatures. Two solutions are generally considered to decrease the temperature: reducing the thickness of the conventional yttria-stabilised zirconia (YSZ) electrolyte and / or using the new materials. The second option seems the most exploitable because novel apatite-type silicates are attracting considerable interest as a new family of oxide-ion conductors with potential use in intermediate temperature between 500 and 800℃. Among the many silicate ceramics that could be used for this application, lanthanum silicates are very promising candidates at the moment.
The objective of this thesis is the synthesis and characterization of apatite-type lanthanum silicate (ATLS) as a novel electrolyte dedicated to SOFC at intermediate temperature (IT-SOFC).
In a first step, this work is to synthesize La_(10)(SiO_4)_6O_3 powders via a solid-state reaction. Particular emphasis is placed on optimizing executive protocols. The control of synthesis parameters (nature reagents, co-grinding, sintering temperatures and residence times, etc.) can get the apatite phase in a sintering temperature between 1350℃and 1650℃. The calcined powders were used to prepare density coatings greater than 90%.
La_(10)(SiO_4))_6O_3 coatings were thermally deposited by conventional atmospheric plasma spraying (APS). The influence of projection parameters on the microstructure of coatings has been studied. The effects of porosity on the electrical properties were also discussed.
Improving the ionic conductivity is based on controlling the properties of developed coatings. For example, several sets of samples to be controlled stoichiometry have been synthesized and characterized. This study has enabled us to establish a correlation between the microstructure and conduction properties of the ceramics.
引文
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[1]Abram EJ,Sinclair DC,West AR.A novel enhancement of ionic conductivity in the cation-deficient apatite La-9.33(SiO4)(6)O-2. Journal of Materials Chemistry 2001; 11: 1978.
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[1]Beauvais S,Guipont V,Borit F,Jeandin M,Espanol M,Khor KA,Robisson A,Saenger R.Process-microstructure-property relationships in controlled atmosphere plasma spraying of ceramics.Surface and Coatings Technology 2004;183:204.
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[1]Abram EJ,Sinclair DC,West AR.A novel enhancement of ionic conductivity in the cation-deficient apatite La-9.33(SiO4)(6)O-2.Journal of Materials Chemistry 2001;11:1978.
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[3]Cedelle J,Vardelle M,Fauchais P.Influence of stainless steel substrate preheating on surface topography and on millimeter-and micrometer-sized splat formation.Surface and Coatings Technology 2006;201:1373.
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[5]Fang JC,Xu W J,Zhao ZY,Zeng HP.In-flight behaviors of ZrO2 particle in plasma spraying.Surface and Coatings Technology 2007;201:5671.
[6]Kim S,Kwon O,Kumar S,Xiong Y,Lee C.Development and microstructure optimization of atmospheric plasma-sprayed NiO/YSZ anode coatings for SOFCs.Surface and Coatings Technology 2008;202:3180.
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[8]Li C-J,Li C-X,Wang M.Effect of spray parameters on the electrical conductivity of plasma-sprayed La1-xSrxMnO3 coating for the cathode of SOFCs.Surface and Coatings Technology 2005;198:278.
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[10]Nakayama S,Higuchi Y,Kondo Y,Sakamoto M.Effects of cation-or oxide ion-defect on conductivities of apatite-type La-Ge-O system ceramics.Solid State Ionics 2004;170:219.
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[12]Nakayama S,Sakamoto M.Electrical properties of new type high oxide ionic conductor RE10Si6027(RE=La,Pr,Nd,Sm,Gd,Dy).Journal of the European Ceramic Society 1998;18:1413.
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[14]Yoshioka H.Oxide ionic conductivity of apatite-type lanthanum silicates.Journal of Alloys and Compounds 2006;408:649.
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[1]Abram EJ,Sinclair DC,West AR.A novel enhancement of ionic conductivity in the cation-deficient apatite La-9.33(SiO4)(6)O-2. Journal of Materials Chemistry 2001; 11: 1978.
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[1]Beauvais S,Guipont V,Borit F,Jeandin M,Espanol M,Khor KA,Robisson A,Saenger R.Process-microstructure-property relationships in controlled atmosphere plasma spraying of ceramics.Surface and Coatings Technology 2004;183:204.
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[1]Abram EJ,Sinclair DC,West AR.A novel enhancement of ionic conductivity in the cation-deficient apatite La-9.33(SiO4)(6)O-2.Journal of Materials Chemistry 2001;11:1978.
[2]Arikawa H,Nishiguchi H,Ishihara T,Takita Y.Oxide ion conductivity in Sr-doped La10Ge6027 apatite oxide.Solid State Ionics 2000;136:31.
[3]Cedelle J,Vardelle M,Fauchais P.Influence of stainless steel substrate preheating on surface topography and on millimeter-and micrometer-sized splat formation.Surface and Coatings Technology 2006;201:1373.
[4]Chefi S,Madani A,Boussetta H,Roux C,Hammou A.Electrical properties of Al-doped oxyapatites at intermediate temperature.Journal of Power Sources 2008;177:464.
[5]Fang JC,Xu W J,Zhao ZY,Zeng HP.In-flight behaviors of ZrO2 particle in plasma spraying.Surface and Coatings Technology 2007;201:5671.
[6]Kim S,Kwon O,Kumar S,Xiong Y,Lee C.Development and microstructure optimization of atmospheric plasma-sprayed NiO/YSZ anode coatings for SOFCs.Surface and Coatings Technology 2008;202:3180.
[7]Kovalevsky AV,Marques FMB,Kharton W,Maxim F,Frade JR.Silica-scavenging effect in zirconia electrolytes:assessment of lanthanum silicate formation.lonics 2006;12:179.
[8]Li C-J,Li C-X,Wang M.Effect of spray parameters on the electrical conductivity of plasma-sprayed La1-xSrxMnO3 coating for the cathode of SOFCs.Surface and Coatings Technology 2005;198:278.
[9]Najib A,Sansom JEH,Tolchard JR,Slater PR,Islam MS.Doping strategies to optimise the oxide ion conductivity in apatite-type ionic conductors.Dalton Transactions 2004:3106.
[10]Nakayama S,Higuchi Y,Kondo Y,Sakamoto M.Effects of cation-or oxide ion-defect on conductivities of apatite-type La-Ge-O system ceramics.Solid State Ionics 2004;170:219.
[11]Nakayama S,Kageyama T,Aono H,Sadaoka Y.Ionic conductivity of lanthanoid silicates,Ln10(SiO4)6O3(Ln=La,Nd,Sm,Gd,Dy,Y,Ho,Er and Yb).Journal of Materials Chemistry 1995;5:1801.
[12]Nakayama S,Sakamoto M.Electrical properties of new type high oxide ionic conductor RE10Si6027(RE=La,Pr,Nd,Sm,Gd,Dy).Journal of the European Ceramic Society 1998;18:1413.
[13]Qunbo F,Lu W,Fuchi W.Modeling influence of basic operation parameters on plasma jet.Journal of Materials Processing Technology 2008;198:207.
[14]Yoshioka H.Oxide ionic conductivity of apatite-type lanthanum silicates.Journal of Alloys and Compounds 2006;408:649.