Y/Gd掺杂与等价元素取代的BaSrCoFeO系SOFC阴极材料性能研究
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摘要
因为能源危机与环境保护两大问题的日益严重，固体氧化物燃料电池（SolidOxide Fuel Cells, SOFC）作为一种高效、清洁的新型发电装置受至研究者的广泛关注。为了降低固体氧化物燃料电池商业化应用的技术难度，需要降低其工作温度，开发在中低温下具有良好性能的阴极材料是在各种降低电池工作温度的途经中有效的方法之一。
本文采用改进的溶胶-凝胶法合成了A位掺小半径稀土元素的(Ba_(0.5)Sr_(0.5))_(1-x)Ln_xCo_(0.8)Fe_(0.2)O_(3-δ)（Ln=Y，Gd；分别简称BSYCFx和BSGCFx）阴极材料，并对两体系材料的系列物性以及电化学性能进行测试。研究结果表明，A位引入小半径稀土元素并没有改变BSCF原有的立方钙钛矿结构。随着稀土掺杂量的增加，晶胞参数变小，由于Y~(3+)离子半径小于Gd~(3+)，BSYCF体系具有比BSGCF体系更小的晶胞体积，并导致BSYCF的热膨胀系数（TEC）高于BSGCF。Y~(3+)与Gd~(3+)部分取代A位离子显著提高了BSCF材料的电导率，随着掺杂量的增多相应的电导率增大，BSYCF20与BSGCF15样品的电导率最大值分别为121.4和148S·cm-1。
对于BSGCF体系，通过对其材料关口尺寸的计算，发现具有最小关口尺寸的BSGCF05样品由于氧离子输运困难而致其在热膨胀性能，热重分析和电导率测试中出现的明显滞后于同系列其他样品的现象，并且导致其扩散系数和扩散活化能最小。热重分析实验结果得到了晶格氧的热解活动规律，它一方面是BSYCF和BSGCF材料热膨胀系数在350-500°C异常膨胀的原因，同时也是材料电导率出现峰值以及变温过程中出现电导弛豫现象的原因。
通过碘滴定反应实验确定了BSCF与BSGCF15阴极材料的在室温下氧含量，结果表明：Gd~(3+)的引入降低B位离子的平均价态，相应的增加B~(3+)/B4+离子的比例，并且当温度升高时，伴随着材料中氧的脱离，氧空位浓度增加，材料中B位离子的平均价态进一步降低，使III价和IV价离子数趋于合理的比例，这是Gd掺杂提高材料电导率以及降低材料阴极扩散阻抗的主要原因。BSGCF15阴极被成功地应用在阳极支撑的SDC薄膜燃料电池上，在600oC电池的最大输出功率密度为551mW·cm~(-2)，开路条件下阴极极化电阻0.16·cm~2。
在发现A位Gd~(3+)掺杂能够明显改善BSCF电化学性能的基础上，我们尝试在A位少量Gd~(3+)掺杂(5%)的基础上改变A位Ba/Sr比例，制备出(Ba_xSr_(1-x))_(0.95)Gd_(0.05)Co_(0.8)Fe_(0.2)O_(3-δ)(0.1≤x≤0.9)阴极材料，重点考察少量Gd掺杂与Ba/Sr比例改变对材料各项性能的影响机制。实验结果表明，(Ba_xSr_(1-x))_(0.95)Gd_(0.05)Co_(0.8)Fe_(0.2)O_(3-δ)(0.1≤x≤0.7)具有立方钙钛矿结构，只有x=0.9的样品伴有少量的BaCoO3杂质，随Ba含量增多晶胞体积膨胀。通过碘滴定反应确定了材料中B位离子价态，结果表明，随着Ba/Sr比例的增加，样品中B位离子的平均价态升高。对材料晶格点阵能进行简单计算的结果显示，和材料中B位离子价态升高而导致材料结构收缩相比，Ba的离子半径大于其它离子半径才是其结构随着Ba/Sr比例的增加所致膨胀的主要原因，同时，为了补偿晶胞膨胀所导致的点阵能下降，B位离子的价态必须升高。Gd掺杂与Ba/Sr比例对材料的热膨胀系数影响不大，材料在50-800°C之间工程膨胀系数（t-TEC）都在20×10~(-6)K~(-1)左右。在5%的Gd掺杂的基础上改变Ba/Sr比例对于材料电导率有显著的影响，电导率随着Ba/Sr比例增加而减少，样品Ba10电导率可以达到σ=298.8S·cm-1。交流阻抗的结果分析表明材料的阻抗值随着Ba/Sr比例变化关系并不是单调的，而随之先增大再减少。在650°C下，x=0.1，_(0.2)，0.3，_(0.5)和0.7的阴极材料的总阻抗Rel分别为0.043，0.061，0.065，0.14和_(0.05)9·cm2。
在A位少量稀土元素Gd的掺杂基础上，改变B位Fe/Co比例得到(Ba_(0.5)Sr_(0.5))_(0.95)Gd_(0.05)Co_(1-x)FexO_(3-δ)（_(0.2)≤x≤1.0）阴极材料，研究其结构，高温热性能，电化学性能等。实验结果表明，(Ba_(0.5)Sr_(0.5))_(0.95)Gd_(0.05)Co_(1-x)FexO_(3-δ)仍具有立方钙钛矿结构，材料的晶胞体积随着Fe含量的增加基本呈减少趋势，但Fe0.4样品具有最大的晶胞常数。材料中B位离子Fe/Co比例改变也并没有使材料的热膨胀系数得到相应的降低，在50-900°C之间其热膨胀系数为20.7-22.4×10-6K-1。热重实验结果表明，随着Fe含量的增加，其在低温区氧化增重的程度明显增加，Fe0.4样品的失重量为最小，这与其具有最小的热膨胀系数相对应。通过对dTG曲线的分析和采用碘滴定法进行的价态测量，区分了材料中B位Co、Fe离子的氧化温区。改变材料中B位Fe/Co比例对于材料电导率的影响不大。随着材料中Fe含量的增加其电导率由64.54S·cm~(-1)减少到21.4S·cm~(-1)。材料的交流阻抗的实验结果表明，Fe0.4样品的电化学性能最好，其阻抗值在650°C为0.07·cm~2。并对Fe0.4在不同氧分压下的阻抗谱进行拟合分析，对于阴极反应机理进行研究。
The energy crisis and environmental development are becoming seriously, Solidoxide fuel cells (SOFCs) as a new kind of chemical device have attracted much attentiondue to their high-energy conversion efficiency and low pollution. With the developmentof practical application research in SOFC, lowering the operation temperature of SOFCsis the key point of the research now. Therefore, the development of new electrodes withhigh electro-catalytic activity for the oxygen-reduction reaction is one effective approachto lower down the operating temperature of SOFC.
Complex oxides of (Ba_(0.5)Sr_(0.5))1xLnxCo_(0.8)Fe_(0.2)O_(3-δ)(Ln=Y, Gd; noted as BSYCFxand BSGCFx) were synthesized via the modified sol-gel method, and their series ofperformances and electrochemical properties were investigated. The results demonstratedthat the rare earth-doped in A-site does not destroy the single phase cubic perovskitestructure of BSCF. With increasing the rare earth-doped content, the lattice constant andunit cell volume shrink. The ion radius of the Y~(3+)is much smaller than that of the Gd~(3+),BSYCF have smaller cell volume and higher thermal expansion coefficient (TEC) thanBSGCF. The Y, Gd-doped greatly improve the electrical conductivity of BSCF. Themaximum conductivities of BSYCF20and BSGCF15are121.4and148S·cm-1.
For BSGCF materials, the rcof BSGCF05is the smallest in all samples, whichmake that the starting temperature of weight loss, the temperature of the abnormalexpansion and the transition temperature of the electrical conductivity for the BSGCF05are higher than those of other samples, and the chemical diffusion coefficient (D~) ofoxygen and the diffusion active energy (Ea) of BSGCF05are the smallest in all samples.The results of thermograimetic measurements (TG) show the action of lattice oxygen,which is a major cause of abnormal expansion, the maximum conductivities at atemperature (350-500°C), and the electrical conductivity relaxation for BSYCF andBSGCF materials.
The oxygen nonstoichiometries of BSCF and BSGCF15tested at room temperatureby the iodometry technique. A larger oxygen nonstoichiometry δ for BSGCF is observeddue to the existence of Gd~(3+)in the A-site. Partial substitution of Ba2+and Sr2+by Gd~(3+)results in the reduction of the valence state in the B-site to maintain the electricalneutrality. The quantity of Co4+and Fe4+in BSGCF is therefore smaller than that ofBSCF. With the increase of temperature, the average valence state in the B-site willcontinue to decrease for the oxygen vacancy concentration increases, which is majorcause that the Gd-doping greatly improves the electrical conductivity and decreases thediffusion resistance of BSCF. The performance of an anode-supported single cell withBSGCF15cathode showed good properties in single-cell. At600°C, the power densitiesis551mW·cm-2, the polarization resistance of cathode is0.16·cm~2.
Then, base on the results of Gd-doped BSCF, we systematically evaluated theeffects of A-site rare earth metal (Gd~(3+)) doping and changing the ratio of Ba/Sr in A-siteon the performance of (Ba_xSr_(1-x))0.95Gd_(0.05)Co_(0.8)Fe_(0.2)O_(3-δ). The samples with x=0.1-0.7have a cubic ABO3perovskite-type structure, except x=0.9with a small amount ofBaCoO3impurity. The lattice parameter increases with doping content of Ba. The oxygennonstoichiometries_(3-δ) and the average valence state in the B-site were enhanced withthe increasing of Ba content from the results of iodometric titration. The crystal latticeenergy calculated results show that the cell expansion is due to the bigger ion radius ofBa2+than that of Sr2+. The Gd-doped and changing the ratio of Ba/Sr slightly reduce thethermal expansion character of BSCF. The thermal expansion coefficient (TEC) is around20×10-6K-1from50-800°C. The Gd-doped and changing the ratio of Ba/Sr greatlyimprove the electrical conductivity of BSCF. The maximum electrical conductivity ofBa10is298.8S·cm-1. the AC impedance results are clearly observed that the totalpolarization resistances (Rel) of (Ba_xSr_(1-x))0.95Gd_(0.05)Co_(0.8)Fe_(0.2)O_(3-δ)show a first increasewith the increasing content of Ba2+(from x=0.1to_(0.5)), reaching a maximum when x=_(0.5), and then a decrease with further increased in content of Ba2+(x=0.7). The Relvaluesare0.043,0.061,0.065,0.14, and_(0.05)9·cm2for x=0.1,_(0.2),0.3,_(0.5), and0.7at650°C,respectively.
In order to ascertain the influence of Gd doping on the properties of the materialfurther, we systematically evaluated the effects of A-site rare earth metal (Gd~(3+)) dopingand changing the ratio of Fe/Co in B-site on the performance of(Ba_(0.5)Sr_(0.5))0.95Gd_(0.05)Co_(1-x)FexO_(3-δ)(_(0.2)≤x≤1.0). The results showed that, the(Ba_(0.5)Sr_(0.5))0.95Gd_(0.05)Co_(1-x)FexO_(3-δ)have a cubic perovskite-type structure, and the latticeparameters firstly increase with increasing Fe-doping amount from x=_(0.2) to0.4, andthen decrease with the further increase of x. The Gd-doped and changing the ratio ofFe/Co slightly reduce the thermal expansion character of BSCF. The thermal expansioncoefficient (TEC) is20.7-22.4×10-6K-1from50-900°C. The results of thermograimeticshowed that weight increase was more significant as Fe concentration increased, and theweight loss and TEC for Fe0.4are the smallest. The results of dTG curves and theaverage valence state in the B-site identify the oxidation temperature range of Fe/Co inB-site. The Gd-doped and changing the ratio of Fe/Co slightly changes the electricalconductivity of BSCF. The maximum electrical conductivities of(Ba_(0.5)Sr_(0.5))0.95Gd_(0.05)Co_(1-x)FexO_(3-δ)have declined from64.54S·cm-1to21.4S·cm-1withincreasing Fe content. Based on the results of the AC impedance, the electrochemistryproperties of Fe0.4are better than others. For example, the impedance of Fe0.4is0.07
·cm2at650°C. To distinguish the individual step of the electrode reaction, impedancespectra of Fe0.4symmetrical cell was measured with oxygen partial pressure from0.022 to0.86atm.
本文采用改进的溶胶-凝胶法合成了A位掺小半径稀土元素的(Ba_(0.5)Sr_(0.5))_(1-x)Ln_xCo_(0.8)Fe_(0.2)O_(3-δ)（Ln=Y，Gd；分别简称BSYCFx和BSGCFx）阴极材料，并对两体系材料的系列物性以及电化学性能进行测试。研究结果表明，A位引入小半径稀土元素并没有改变BSCF原有的立方钙钛矿结构。随着稀土掺杂量的增加，晶胞参数变小，由于Y~(3+)离子半径小于Gd~(3+)，BSYCF体系具有比BSGCF体系更小的晶胞体积，并导致BSYCF的热膨胀系数（TEC）高于BSGCF。Y~(3+)与Gd~(3+)部分取代A位离子显著提高了BSCF材料的电导率，随着掺杂量的增多相应的电导率增大，BSYCF20与BSGCF15样品的电导率最大值分别为121.4和148S·cm-1。
对于BSGCF体系，通过对其材料关口尺寸的计算，发现具有最小关口尺寸的BSGCF05样品由于氧离子输运困难而致其在热膨胀性能，热重分析和电导率测试中出现的明显滞后于同系列其他样品的现象，并且导致其扩散系数和扩散活化能最小。热重分析实验结果得到了晶格氧的热解活动规律，它一方面是BSYCF和BSGCF材料热膨胀系数在350-500°C异常膨胀的原因，同时也是材料电导率出现峰值以及变温过程中出现电导弛豫现象的原因。
通过碘滴定反应实验确定了BSCF与BSGCF15阴极材料的在室温下氧含量，结果表明：Gd~(3+)的引入降低B位离子的平均价态，相应的增加B~(3+)/B4+离子的比例，并且当温度升高时，伴随着材料中氧的脱离，氧空位浓度增加，材料中B位离子的平均价态进一步降低，使III价和IV价离子数趋于合理的比例，这是Gd掺杂提高材料电导率以及降低材料阴极扩散阻抗的主要原因。BSGCF15阴极被成功地应用在阳极支撑的SDC薄膜燃料电池上，在600oC电池的最大输出功率密度为551mW·cm~(-2)，开路条件下阴极极化电阻0.16·cm~2。
在发现A位Gd~(3+)掺杂能够明显改善BSCF电化学性能的基础上，我们尝试在A位少量Gd~(3+)掺杂(5%)的基础上改变A位Ba/Sr比例，制备出(Ba_xSr_(1-x))_(0.95)Gd_(0.05)Co_(0.8)Fe_(0.2)O_(3-δ)(0.1≤x≤0.9)阴极材料，重点考察少量Gd掺杂与Ba/Sr比例改变对材料各项性能的影响机制。实验结果表明，(Ba_xSr_(1-x))_(0.95)Gd_(0.05)Co_(0.8)Fe_(0.2)O_(3-δ)(0.1≤x≤0.7)具有立方钙钛矿结构，只有x=0.9的样品伴有少量的BaCoO3杂质，随Ba含量增多晶胞体积膨胀。通过碘滴定反应确定了材料中B位离子价态，结果表明，随着Ba/Sr比例的增加，样品中B位离子的平均价态升高。对材料晶格点阵能进行简单计算的结果显示，和材料中B位离子价态升高而导致材料结构收缩相比，Ba的离子半径大于其它离子半径才是其结构随着Ba/Sr比例的增加所致膨胀的主要原因，同时，为了补偿晶胞膨胀所导致的点阵能下降，B位离子的价态必须升高。Gd掺杂与Ba/Sr比例对材料的热膨胀系数影响不大，材料在50-800°C之间工程膨胀系数（t-TEC）都在20×10~(-6)K~(-1)左右。在5%的Gd掺杂的基础上改变Ba/Sr比例对于材料电导率有显著的影响，电导率随着Ba/Sr比例增加而减少，样品Ba10电导率可以达到σ=298.8S·cm-1。交流阻抗的结果分析表明材料的阻抗值随着Ba/Sr比例变化关系并不是单调的，而随之先增大再减少。在650°C下，x=0.1，_(0.2)，0.3，_(0.5)和0.7的阴极材料的总阻抗Rel分别为0.043，0.061，0.065，0.14和_(0.05)9·cm2。
在A位少量稀土元素Gd的掺杂基础上，改变B位Fe/Co比例得到(Ba_(0.5)Sr_(0.5))_(0.95)Gd_(0.05)Co_(1-x)FexO_(3-δ)（_(0.2)≤x≤1.0）阴极材料，研究其结构，高温热性能，电化学性能等。实验结果表明，(Ba_(0.5)Sr_(0.5))_(0.95)Gd_(0.05)Co_(1-x)FexO_(3-δ)仍具有立方钙钛矿结构，材料的晶胞体积随着Fe含量的增加基本呈减少趋势，但Fe0.4样品具有最大的晶胞常数。材料中B位离子Fe/Co比例改变也并没有使材料的热膨胀系数得到相应的降低，在50-900°C之间其热膨胀系数为20.7-22.4×10-6K-1。热重实验结果表明，随着Fe含量的增加，其在低温区氧化增重的程度明显增加，Fe0.4样品的失重量为最小，这与其具有最小的热膨胀系数相对应。通过对dTG曲线的分析和采用碘滴定法进行的价态测量，区分了材料中B位Co、Fe离子的氧化温区。改变材料中B位Fe/Co比例对于材料电导率的影响不大。随着材料中Fe含量的增加其电导率由64.54S·cm~(-1)减少到21.4S·cm~(-1)。材料的交流阻抗的实验结果表明，Fe0.4样品的电化学性能最好，其阻抗值在650°C为0.07·cm~2。并对Fe0.4在不同氧分压下的阻抗谱进行拟合分析，对于阴极反应机理进行研究。
The energy crisis and environmental development are becoming seriously, Solidoxide fuel cells (SOFCs) as a new kind of chemical device have attracted much attentiondue to their high-energy conversion efficiency and low pollution. With the developmentof practical application research in SOFC, lowering the operation temperature of SOFCsis the key point of the research now. Therefore, the development of new electrodes withhigh electro-catalytic activity for the oxygen-reduction reaction is one effective approachto lower down the operating temperature of SOFC.
Complex oxides of (Ba_(0.5)Sr_(0.5))1xLnxCo_(0.8)Fe_(0.2)O_(3-δ)(Ln=Y, Gd; noted as BSYCFxand BSGCFx) were synthesized via the modified sol-gel method, and their series ofperformances and electrochemical properties were investigated. The results demonstratedthat the rare earth-doped in A-site does not destroy the single phase cubic perovskitestructure of BSCF. With increasing the rare earth-doped content, the lattice constant andunit cell volume shrink. The ion radius of the Y~(3+)is much smaller than that of the Gd~(3+),BSYCF have smaller cell volume and higher thermal expansion coefficient (TEC) thanBSGCF. The Y, Gd-doped greatly improve the electrical conductivity of BSCF. Themaximum conductivities of BSYCF20and BSGCF15are121.4and148S·cm-1.
For BSGCF materials, the rcof BSGCF05is the smallest in all samples, whichmake that the starting temperature of weight loss, the temperature of the abnormalexpansion and the transition temperature of the electrical conductivity for the BSGCF05are higher than those of other samples, and the chemical diffusion coefficient (D~) ofoxygen and the diffusion active energy (Ea) of BSGCF05are the smallest in all samples.The results of thermograimetic measurements (TG) show the action of lattice oxygen,which is a major cause of abnormal expansion, the maximum conductivities at atemperature (350-500°C), and the electrical conductivity relaxation for BSYCF andBSGCF materials.
The oxygen nonstoichiometries of BSCF and BSGCF15tested at room temperatureby the iodometry technique. A larger oxygen nonstoichiometry δ for BSGCF is observeddue to the existence of Gd~(3+)in the A-site. Partial substitution of Ba2+and Sr2+by Gd~(3+)results in the reduction of the valence state in the B-site to maintain the electricalneutrality. The quantity of Co4+and Fe4+in BSGCF is therefore smaller than that ofBSCF. With the increase of temperature, the average valence state in the B-site willcontinue to decrease for the oxygen vacancy concentration increases, which is majorcause that the Gd-doping greatly improves the electrical conductivity and decreases thediffusion resistance of BSCF. The performance of an anode-supported single cell withBSGCF15cathode showed good properties in single-cell. At600°C, the power densitiesis551mW·cm-2, the polarization resistance of cathode is0.16·cm~2.
Then, base on the results of Gd-doped BSCF, we systematically evaluated theeffects of A-site rare earth metal (Gd~(3+)) doping and changing the ratio of Ba/Sr in A-siteon the performance of (Ba_xSr_(1-x))0.95Gd_(0.05)Co_(0.8)Fe_(0.2)O_(3-δ). The samples with x=0.1-0.7have a cubic ABO3perovskite-type structure, except x=0.9with a small amount ofBaCoO3impurity. The lattice parameter increases with doping content of Ba. The oxygennonstoichiometries_(3-δ) and the average valence state in the B-site were enhanced withthe increasing of Ba content from the results of iodometric titration. The crystal latticeenergy calculated results show that the cell expansion is due to the bigger ion radius ofBa2+than that of Sr2+. The Gd-doped and changing the ratio of Ba/Sr slightly reduce thethermal expansion character of BSCF. The thermal expansion coefficient (TEC) is around20×10-6K-1from50-800°C. The Gd-doped and changing the ratio of Ba/Sr greatlyimprove the electrical conductivity of BSCF. The maximum electrical conductivity ofBa10is298.8S·cm-1. the AC impedance results are clearly observed that the totalpolarization resistances (Rel) of (Ba_xSr_(1-x))0.95Gd_(0.05)Co_(0.8)Fe_(0.2)O_(3-δ)show a first increasewith the increasing content of Ba2+(from x=0.1to_(0.5)), reaching a maximum when x=_(0.5), and then a decrease with further increased in content of Ba2+(x=0.7). The Relvaluesare0.043,0.061,0.065,0.14, and_(0.05)9·cm2for x=0.1,_(0.2),0.3,_(0.5), and0.7at650°C,respectively.
In order to ascertain the influence of Gd doping on the properties of the materialfurther, we systematically evaluated the effects of A-site rare earth metal (Gd~(3+)) dopingand changing the ratio of Fe/Co in B-site on the performance of(Ba_(0.5)Sr_(0.5))0.95Gd_(0.05)Co_(1-x)FexO_(3-δ)(_(0.2)≤x≤1.0). The results showed that, the(Ba_(0.5)Sr_(0.5))0.95Gd_(0.05)Co_(1-x)FexO_(3-δ)have a cubic perovskite-type structure, and the latticeparameters firstly increase with increasing Fe-doping amount from x=_(0.2) to0.4, andthen decrease with the further increase of x. The Gd-doped and changing the ratio ofFe/Co slightly reduce the thermal expansion character of BSCF. The thermal expansioncoefficient (TEC) is20.7-22.4×10-6K-1from50-900°C. The results of thermograimeticshowed that weight increase was more significant as Fe concentration increased, and theweight loss and TEC for Fe0.4are the smallest. The results of dTG curves and theaverage valence state in the B-site identify the oxidation temperature range of Fe/Co inB-site. The Gd-doped and changing the ratio of Fe/Co slightly changes the electricalconductivity of BSCF. The maximum electrical conductivities of(Ba_(0.5)Sr_(0.5))0.95Gd_(0.05)Co_(1-x)FexO_(3-δ)have declined from64.54S·cm-1to21.4S·cm-1withincreasing Fe content. Based on the results of the AC impedance, the electrochemistryproperties of Fe0.4are better than others. For example, the impedance of Fe0.4is0.07
·cm2at650°C. To distinguish the individual step of the electrode reaction, impedancespectra of Fe0.4symmetrical cell was measured with oxygen partial pressure from0.022 to0.86atm.
引文
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