中温H_2S固体氧化物燃料电池阳极材料的制备及性能研究
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摘要
基于国内外固体氧化物燃料电池(SOFC)的发展,针对其在高温及H2S燃气下的局限性,论文以中温H2S SOFC阳极材料为研究对象,采用实验与热力学软件分析相结合的方法,系统地研究了几种阳极材料的制备方法及其电化学性能,并构建以电解质为支撑的单电池,通过测试其电输出性能,筛选出最适合中温H2S SOFC的阳极材料。
采用尿素燃烧法制备了不同掺杂量的钙钛矿结构Lao7Sr0.3Cr1-xYxO3-δ(简写为LSCY阳极材料。经X-射线衍射(XRD).H2S电导率及H2-程序升温还原(H2-TPR)测试确定了LSCY的最适煅烧温度为1350℃、Y的最佳掺杂量为0.13、催化活性温度为600℃。以氧离子型Ce0.8Sm0.2O1.9(SDC)电解质为支撑,构建单电池LSCY13-SDC‖SDC‖Ag,在600℃及5%H2S燃气下,开路电压为0.85V,最大功率密度为12.42mW·cm-2.单电池运行前后阳极材料的X射线光电子能谱(XPS)及光致发光光谱(PL)表征结果表明,Sr取代La后产生不带电的氧空位,为O2-传导提供了通道,扩大了H2S与O2-反应三相界面；Y掺杂后由于体系中存在离域的d电子,增强了该阳极材料的电子电导性。
采用溶胶燃烧法制备了Ce0.9Sr0.1Cr0.5Co0.5O4-δ(CSCCo)的前驱体粉末,1100℃及3%H2条件下还原5h得到萤石结构的CSCCo阳极材料。经XRD、H2-TPR及FT-IR等测试,结果表明CSCCo适合作为中温H2S SOFC的阳极材料。构建的CSCCo-SDC‖SDC‖Ag单电池,在600℃及5%H2S燃气下,开路电压为0.97V,最大功率密度为14.21mW·cm-2.单电池运行前后阳极材料的XPS测试表明,Ce3+的电子容易跃迁到Co3+上,电子的这种跃迁增强了阳极材料的电子电导性；生成的H20与阳极表面的氧空位作用产生羟基氧,其易与H2S中的H发生作用,提高了单电池在H2S燃气中的电输出性能。
采用溶胶燃烧法制备了Ce0.9Sr0.1Cr0.5Mn0.5O4-δ(CSCMn)前驱体粉末,在1100℃及3%H2条件下还原5h得到萤石结构的CSCMn阳极材料。经XRD、H2-TPR及H2S电导率等测试,确定CSCMn粉末适合作为中温H2S SOFC的阳极材料。构建的CSCMn-SDC‖SDC‖Ag单电池,在600℃及5%H2S燃气下,开路电压和最大功率密度分别为0.95V和15.12mW·cm-2.单电池运行前后阳极材料的XPS谱图表明,CSCMn体系中存在Ce3+电子跃迁至Mn4+上,电子的这种跃迁增大了材料的电子电导性；阳极表面的晶格氧转化为化学间隙氧,同时放出的氧空位把来自阴极的O2-传导到阳极材料表面,扩大了H2S与O2-反应的三相界面,提高了单电池的电输出性能。
采用溶胶燃烧法制备了Ce0.9Sr0.1Cr0.5Fe0.5O3-δ(CSCFe)前驱体粉末,经3%H2和100%H2还原分别得到钙钛矿结构和萤石结构的CSCFe阳极材料,通过XRD.H2-TPR及FT-IR等测试表明,二者均适合作为中温H2S SOFC的阳极材料,由此构建的单电池CSCMn-SDC‖SDC‖Ag在600℃及5%H2S燃气下,其最大电流密度分别为52.35mA·cm·-2和82.38mA.cm-2,最大功率密度分别为17.75mW.cm-2和18.75mW.cm-2,表明钙钛矿结构的CSCFe阳极材料比萤石结构的催化活性要低一些,这是由于这两种CSCFe材料中Ce3+含量不同所引起的,前者Ce3+的含量(30.35%)比后者的(70.26%)要低的多。
以质子型电解质BaCe0.35Zr0.5Y0.15O3-δ(BCZY)为支撑,分别以无定形结构的BaCe0.35Zr0.5Y0.15O3-Li3PO4-CaSO4(BCZY-Li-Ca)和钙钛矿结构的Ce0.8Sr0.2Cr0.5V0.5O3-δ (CSCV)为阳极材料,构建的单电池BCZY-Li-Ca-BCZY‖BCZY‖Ag和CSCV-BCZY‖BCZY‖Ag,在600℃及5%H2S燃气下,开路电压分别为0.81V和0.99V,最大功率密度分别为13.1mW·cm-2和22.6mW·cm-2。CSCV阳极材料和BCZY电解质同为钙钛矿结构且.均含有Ce,因而二者的化学相容性更好,同时降低了其接触电阻,导致单电池的电性能输出更好。
Based on the development of higher temperature H2S Solid Oxide Fuel Cells (SOFC), in order to overcome the shortcoming of the materials under the condition of higher temperature and in H2S, the paper was focused on anode materials for intermediate temperature H2S SOFC by experiments and analysis of thermodynamic calculation. The preparations of sevrial anode and the properties of them in H2S were studied. After building single cells which electrolytes as surppoted, the tested electrochemical properties were used to find out a more suitable anode for intermediate temperature H2S SOFC.
Urea combustion method was used to prepare a series of La0.7Sr0.3Cr1-xYx03-δ (abbreviation:LSCY). The measurements of X-ray diffraction (XRD), conductivities in H2S and H2-temperature programmed reduction (H2-TPR) were used to determine the optimum sintering temperature1350℃and the favourable doping quantity x=0.13. The maximum OCV was0.85V and the maximum power density was12.42mW·cm-2for the single cell LSCY13-SDC‖SDC‖Ag in5%H2S at600℃. The results of X-ray photoelectron spectroscopy (XPS) and Photoluminescence (PL) after the cell test showed that La was replaced by Sr to produce oxygen vacancies which had no charge, and the oxygen vacancies provided channel for migrating of O2-, which enlarged area of reaction H2S with O2-. The appearance of delocalized d electron after Y doping enhanced the conduction of the anode material.
Gel combustion method was used to synthesize Ce0.9Sr0.1Cr0.5Co0.5O4-δ (CSCCo) precursor, then reduced in3%H2at1100℃to get fluorite of CSCCo anode powder. The results of XRD, H2-TPR and FT-IR, et al. showed that CSCCo was suit for as anode for intermediate temperature H2S SOFC. The maximum OCV was0.97V and the maximum power density was14.21mW·cm-2for the single cell CSCCo-SDC‖SDC‖Ag in5%H2S at600℃. Due to the electron easily transfering from Ce3+to Co3+, the hoping elentron increased the electron conductivity of the material; meanwhile Sr doping producing oxygen vacancies was in favour of enhancing the electrochemical properties for intermediate temperature H2S SOFC.
Ce0.9Sr0.1Cr0.5Mn0.5O4-δ (CSCMn) precursor was synthesized by gel combustion method, after reduction in3%H2, the fluorite of CSCMn anode powder was abtained. The analysis of XRD、H2-TPR and conductiviyies in H2S made sure CSCMn fitting as anode for intermediate temperature H2S SOFC. The maximum OCV was0.95V and the maximum power density was15.12mW·cm-2for the single cell CSCMn-SDC‖SDC‖Ag in5%H2S at600℃. After the single cell test, XPS patterns showed that electron transferred from Ce3+to Mn4+which enhanced the conduction of the anode material. Lattice oxygen on the surface of the anode was changed to interstitial atom of oxygen and letted out oxygen vacancies, which magnified the area of touching for H2S and O2-.
Gel combustion method was used to synthesize Ce0.9Sr0.1Cr0.5Fe0.5O3-δ(CSCFe) precursor powder, perovskite CSCFe and fluorite type CSCFe were gotten after the reducrion in3%H2or in100%H2at1100℃for5h. XRD, H2-TPR and FT-IR were used to certain both CSCFe all suiting as anodes for intermediate temperature of H2S SOFC, and the single with them as anode, the maximum current densities were52.35mA·cm-2and82.38mA·cm-2, the maximum power densities were17.75mW·cm-2and18.75mW·cm-2for the cell CSCFe-SDC‖SDC‖Ag in5%H2S at600℃, respectively. The reason may be the difference from content of Ce3+in CSCFe; Ce3+in the former (30.35%) was less than the latter (70.26%).
Model of the cell was proton conducting electrolyte BaCe0.35Zr0.5Y0.15O3-δ as supported. Amorphous structure BaCe0.35Zr0.5Y0.15O3-Li3PO4-CaSO4(BCZY-Li-Ca) and perovskite structure Ce0.8Sr0.2Cr0.5V0.5O3-δ(CSCV) as anode, the electrochemical propteries were carried out for the single cells BCZY-Li-Ca-BCZY‖BCZY‖Ag and CSCV8255-BCZY‖BCZY‖Ag in5%H2S at600℃, the maximum OCVs were0.81V and0.99V, the maximum power densities were13.1mW·cm-2and22.6mW·cm-2, respectively. The activity of fomer was lower than that of the former, the reason was that CSCV and BCZY were all perovskite and all contained Ce, which made magnify the chemical compatibility and reduced the contacting resisitance between them.
采用尿素燃烧法制备了不同掺杂量的钙钛矿结构Lao7Sr0.3Cr1-xYxO3-δ(简写为LSCY阳极材料。经X-射线衍射(XRD).H2S电导率及H2-程序升温还原(H2-TPR)测试确定了LSCY的最适煅烧温度为1350℃、Y的最佳掺杂量为0.13、催化活性温度为600℃。以氧离子型Ce0.8Sm0.2O1.9(SDC)电解质为支撑,构建单电池LSCY13-SDC‖SDC‖Ag,在600℃及5%H2S燃气下,开路电压为0.85V,最大功率密度为12.42mW·cm-2.单电池运行前后阳极材料的X射线光电子能谱(XPS)及光致发光光谱(PL)表征结果表明,Sr取代La后产生不带电的氧空位,为O2-传导提供了通道,扩大了H2S与O2-反应三相界面；Y掺杂后由于体系中存在离域的d电子,增强了该阳极材料的电子电导性。
采用溶胶燃烧法制备了Ce0.9Sr0.1Cr0.5Co0.5O4-δ(CSCCo)的前驱体粉末,1100℃及3%H2条件下还原5h得到萤石结构的CSCCo阳极材料。经XRD、H2-TPR及FT-IR等测试,结果表明CSCCo适合作为中温H2S SOFC的阳极材料。构建的CSCCo-SDC‖SDC‖Ag单电池,在600℃及5%H2S燃气下,开路电压为0.97V,最大功率密度为14.21mW·cm-2.单电池运行前后阳极材料的XPS测试表明,Ce3+的电子容易跃迁到Co3+上,电子的这种跃迁增强了阳极材料的电子电导性；生成的H20与阳极表面的氧空位作用产生羟基氧,其易与H2S中的H发生作用,提高了单电池在H2S燃气中的电输出性能。
采用溶胶燃烧法制备了Ce0.9Sr0.1Cr0.5Mn0.5O4-δ(CSCMn)前驱体粉末,在1100℃及3%H2条件下还原5h得到萤石结构的CSCMn阳极材料。经XRD、H2-TPR及H2S电导率等测试,确定CSCMn粉末适合作为中温H2S SOFC的阳极材料。构建的CSCMn-SDC‖SDC‖Ag单电池,在600℃及5%H2S燃气下,开路电压和最大功率密度分别为0.95V和15.12mW·cm-2.单电池运行前后阳极材料的XPS谱图表明,CSCMn体系中存在Ce3+电子跃迁至Mn4+上,电子的这种跃迁增大了材料的电子电导性；阳极表面的晶格氧转化为化学间隙氧,同时放出的氧空位把来自阴极的O2-传导到阳极材料表面,扩大了H2S与O2-反应的三相界面,提高了单电池的电输出性能。
采用溶胶燃烧法制备了Ce0.9Sr0.1Cr0.5Fe0.5O3-δ(CSCFe)前驱体粉末,经3%H2和100%H2还原分别得到钙钛矿结构和萤石结构的CSCFe阳极材料,通过XRD.H2-TPR及FT-IR等测试表明,二者均适合作为中温H2S SOFC的阳极材料,由此构建的单电池CSCMn-SDC‖SDC‖Ag在600℃及5%H2S燃气下,其最大电流密度分别为52.35mA·cm·-2和82.38mA.cm-2,最大功率密度分别为17.75mW.cm-2和18.75mW.cm-2,表明钙钛矿结构的CSCFe阳极材料比萤石结构的催化活性要低一些,这是由于这两种CSCFe材料中Ce3+含量不同所引起的,前者Ce3+的含量(30.35%)比后者的(70.26%)要低的多。
以质子型电解质BaCe0.35Zr0.5Y0.15O3-δ(BCZY)为支撑,分别以无定形结构的BaCe0.35Zr0.5Y0.15O3-Li3PO4-CaSO4(BCZY-Li-Ca)和钙钛矿结构的Ce0.8Sr0.2Cr0.5V0.5O3-δ (CSCV)为阳极材料,构建的单电池BCZY-Li-Ca-BCZY‖BCZY‖Ag和CSCV-BCZY‖BCZY‖Ag,在600℃及5%H2S燃气下,开路电压分别为0.81V和0.99V,最大功率密度分别为13.1mW·cm-2和22.6mW·cm-2。CSCV阳极材料和BCZY电解质同为钙钛矿结构且.均含有Ce,因而二者的化学相容性更好,同时降低了其接触电阻,导致单电池的电性能输出更好。
Based on the development of higher temperature H2S Solid Oxide Fuel Cells (SOFC), in order to overcome the shortcoming of the materials under the condition of higher temperature and in H2S, the paper was focused on anode materials for intermediate temperature H2S SOFC by experiments and analysis of thermodynamic calculation. The preparations of sevrial anode and the properties of them in H2S were studied. After building single cells which electrolytes as surppoted, the tested electrochemical properties were used to find out a more suitable anode for intermediate temperature H2S SOFC.
Urea combustion method was used to prepare a series of La0.7Sr0.3Cr1-xYx03-δ (abbreviation:LSCY). The measurements of X-ray diffraction (XRD), conductivities in H2S and H2-temperature programmed reduction (H2-TPR) were used to determine the optimum sintering temperature1350℃and the favourable doping quantity x=0.13. The maximum OCV was0.85V and the maximum power density was12.42mW·cm-2for the single cell LSCY13-SDC‖SDC‖Ag in5%H2S at600℃. The results of X-ray photoelectron spectroscopy (XPS) and Photoluminescence (PL) after the cell test showed that La was replaced by Sr to produce oxygen vacancies which had no charge, and the oxygen vacancies provided channel for migrating of O2-, which enlarged area of reaction H2S with O2-. The appearance of delocalized d electron after Y doping enhanced the conduction of the anode material.
Gel combustion method was used to synthesize Ce0.9Sr0.1Cr0.5Co0.5O4-δ (CSCCo) precursor, then reduced in3%H2at1100℃to get fluorite of CSCCo anode powder. The results of XRD, H2-TPR and FT-IR, et al. showed that CSCCo was suit for as anode for intermediate temperature H2S SOFC. The maximum OCV was0.97V and the maximum power density was14.21mW·cm-2for the single cell CSCCo-SDC‖SDC‖Ag in5%H2S at600℃. Due to the electron easily transfering from Ce3+to Co3+, the hoping elentron increased the electron conductivity of the material; meanwhile Sr doping producing oxygen vacancies was in favour of enhancing the electrochemical properties for intermediate temperature H2S SOFC.
Ce0.9Sr0.1Cr0.5Mn0.5O4-δ (CSCMn) precursor was synthesized by gel combustion method, after reduction in3%H2, the fluorite of CSCMn anode powder was abtained. The analysis of XRD、H2-TPR and conductiviyies in H2S made sure CSCMn fitting as anode for intermediate temperature H2S SOFC. The maximum OCV was0.95V and the maximum power density was15.12mW·cm-2for the single cell CSCMn-SDC‖SDC‖Ag in5%H2S at600℃. After the single cell test, XPS patterns showed that electron transferred from Ce3+to Mn4+which enhanced the conduction of the anode material. Lattice oxygen on the surface of the anode was changed to interstitial atom of oxygen and letted out oxygen vacancies, which magnified the area of touching for H2S and O2-.
Gel combustion method was used to synthesize Ce0.9Sr0.1Cr0.5Fe0.5O3-δ(CSCFe) precursor powder, perovskite CSCFe and fluorite type CSCFe were gotten after the reducrion in3%H2or in100%H2at1100℃for5h. XRD, H2-TPR and FT-IR were used to certain both CSCFe all suiting as anodes for intermediate temperature of H2S SOFC, and the single with them as anode, the maximum current densities were52.35mA·cm-2and82.38mA·cm-2, the maximum power densities were17.75mW·cm-2and18.75mW·cm-2for the cell CSCFe-SDC‖SDC‖Ag in5%H2S at600℃, respectively. The reason may be the difference from content of Ce3+in CSCFe; Ce3+in the former (30.35%) was less than the latter (70.26%).
Model of the cell was proton conducting electrolyte BaCe0.35Zr0.5Y0.15O3-δ as supported. Amorphous structure BaCe0.35Zr0.5Y0.15O3-Li3PO4-CaSO4(BCZY-Li-Ca) and perovskite structure Ce0.8Sr0.2Cr0.5V0.5O3-δ(CSCV) as anode, the electrochemical propteries were carried out for the single cells BCZY-Li-Ca-BCZY‖BCZY‖Ag and CSCV8255-BCZY‖BCZY‖Ag in5%H2S at600℃, the maximum OCVs were0.81V and0.99V, the maximum power densities were13.1mW·cm-2and22.6mW·cm-2, respectively. The activity of fomer was lower than that of the former, the reason was that CSCV and BCZY were all perovskite and all contained Ce, which made magnify the chemical compatibility and reduced the contacting resisitance between them.
引文
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