EB-PVD工艺制备YSZ及Ni-YSZ功能涂层的研究
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摘要
本文采用电子束物理气相沉积(EB-PVD)技术制备了用于固体氧化物燃料电池(SOFC)的Ni-YSZ阳极涂层及YSZ电解质涂层材料。采用X射线荧光光谱(XRF)、X射线衍射(XRD)、扫描电镜(SEM)、电子探针(EPMA)、透射电镜(TEM)、原子力显微镜等分析测试技术对涂层的成分及微观组织结构进行了研究,对涂层的孔隙率、气密性及电导率等性能进行了测试和表征,并对组装的单电池的输出性能进行了研究。
采用EB-PVD工艺在多孔的NiO-YSZ基体上制备了8YSZ电解质涂层,制备态及1000°C退火后的涂层均由单一的立方YSZ相组成。电解质涂层的SEM分析表明,涂层呈现出典型的柱状晶结构,在柱状晶间隙处存在微米级的孔隙。涂层元素沿断面分布的EPMA分析结果表明,涂层内的Zr、Y、O元素分布均匀。TEM分析结果表明,涂层的断面由条形或锥形的晶粒组成,在这些晶粒的内部呈现出许多宽度为几纳米并按照一定角度倾斜的白色迹线。
气密性测试结果表明,EB-PVD工艺制备的YSZ电解质涂层的气体扩散系数为9.78×10-5 cm4·N-1·s-1,此值较大气等离子喷涂制得的电解质涂层的气体扩散系数降低了60%以上。YSZ电解质涂层的电导率表现出显著的各向异性,在500°C~800°C的温度范围内,电解质涂层垂直于涂层表面方向的电导率均显著高于平行于表面方向的电导率。根据Arrhenius方程计算出的垂直于涂层表面方向和平行于涂层表面方向的电导活化能分别为80.884kJ/mol和110.147kJ/mol。采用低压浸渗装置对EB-PVD制备的电解质涂层进行了溶胶浸渗处理,根据对溶胶前驱体粉末进行的DSC-TG分析和XRD分析结果确定了致密化的烧结工艺。经过溶胶浸渗处理之后,电解质涂层的气体扩散系数从制备态的9.78×10-5 cm4·N-1·s-1下降至4次和8次溶胶浸渗处理后的3.18×10-5 cm4·N-1·s-1和9.56×10-6 cm4·N-1·s-1。SEM分析表明,溶胶浸渗处理之后,制备态电解质涂层表面晶体颗粒之间的孔隙和缺陷被溶胶所填充,涂层表面变得光滑、致密;断面分析表明,溶胶渗入涂层的深度可达3.5μm。相对于制备态涂层材料的电导率,经过4次和8次溶胶浸渗处理之后,垂直于涂层表面方向电导率提高的幅度均在10%以内,且8次浸渗处理相对4次浸渗处理之后涂层电导率的提高不明显。溶胶浸渗处理后8YSZ电解质涂层垂直于涂层表面的电导率仍比块体材料电导率低30%左右。
单电池800°C的输出性能表明,采用制备态YSZ涂层作为电解质材料的单电池其开路电压为0.820V,采用经过4次和8次溶胶浸渗处理后的涂层作为电解质材料的单电池,其开路电压分别升高至1.017V和1.036V。对于采用制备态电解质涂层的单电池,其最大输出功率密度为70mW/cm2;电解质涂层经过4次和8次浸渗处理后,单电池的最大输出功率密度分别提高到为140mW/cm2和153 mW/cm2。
与此同时,采用双源蒸发工艺,通过同时蒸发金属Ni和YSZ锭料沉积制备了Ni-YSZ涂层。SEM分析表明,Ni-YSZ涂层表现为典型的柱状晶生长模式。TEM分析表明涂层内的晶粒细小且含有大量纳米级的孔隙。N2吸附曲线结果表明,涂层的比表面积为3.232m2/g,平均孔径为25nm,总的孔体积为0.0202cm3/g。由于第二相粒子的加入对阴影效应的强化作用,当Ni含量由18%增加至44%时,Ni-YSZ涂层的孔隙率亦由12%增长至19%;当Ni含量进一步增长至63%,涂层的孔隙率呈现出下降趋势,由19%下降至11%。随着Ni含量的变化,Ni-YSZ涂层的电导率表现出了典型的S形曲线。
采用双源蒸发工艺,通过同时蒸发NiO和YSZ锭料沉积制备了NiO-YSZ涂层,并在800oC氢气气氛下还原2h得到最终的Ni-YSZ涂层。SEM分析表明涂层的孔隙直径大部分在几十纳米到几百纳米范围内。相对于直接利用EB-PVD工艺制备的Ni-YSZ涂层,NiO-YSZ涂层经过还原处理得到的Ni-YSZ涂层,其比表面积由3.232m2/g提高到4.330m2/g,总的孔隙体积由0.02024cm3/g提高到0.03460cm3/g。通过对电子束流的控制,成功制备出了一种成分及孔隙率均沿断面连续变化的梯度涂层,涂层在靠近基板一侧孔隙率及孔隙直径较大,而在靠近表面一侧涂层的孔隙直径以及孔隙率均明显变小。在采用上述方法制得NiO-YSZ阳极涂层的基础上,关闭用于蒸发NiO的电子束电流,通过连续沉积制备了YSZ电解质涂层,实现了SOFC阳极及电解质涂层的连续沉积。
Electron beam physical vapor deposition (EB-PVD) technique was employed to prepare the Ni-YSZ anode coatings as well as the YSZ electrolyte coatings for SOFCs in this study. The chemical composition and microstructure of the coatings were analyzed by x-ray fluorescence spectra (XRF), x-ray diffraction (XRD), scanning electron microscope (SEM), electron probe mciroanalysis (EPMA), transmitting electron microscope (TEM), and atom force microscope (AFM). Then the properties of these coatings, such as porosity, gas tightness, electrical conductivity and so on, were measured and characterized. At the same time, unit cells were assembled and output performances were investigated.
8YSZ electrolyte coatings were prepared by EB-PVD process on porous NiO-YSZ substrates. Both the as-deposited coating and the coating annealed at 1000°C consisted of a single phase of cubic YSZ. SEM analysis demonstrated that electrolyte coating exhibited a characteristic columnar structure. In gaps between the columns, there were many pores with the magnitude of micrometers. A uniform distribution of zirconium, yttrium and oxygen was realized along the direction across coating thickness according to EPMA. TEM analysis indicated that there were many crystalline grains with shapes of strip and pyramid in coating cross-section. Many white lines, with the width of several nanometers, appeared within these grains and inclined with some angle.
Gas-tightness measurement results demonstrated that a gas permeability of 9.78×10-5 cm4·N-1·s-1 was obtained for YSZ electrolyte prepared by EB-PVD, which was lower than that of electrolyte coating prepared by atmosphere plasma spraying by 60%. The electrical conductivity of YSZ electrolyte coating exhibited a typical anisotropy. In temperature range of 500°C~800°C, the electrical conductivity in direction perpendicular to coating surface was obviously higher that in direction parallel to coating surface. According to Arrhenius equation, activation energies for electrical conduction in the directions both perpendicular and parallel to coating surface were 80.884kJ/mol and 110.147kJ/mol respectively.
A sol infiltration device at subatmospheric pressure was used to densify the YSZ electrolyte coatings. Then the post-sintering process was determined according to the analysis results of DSC-TG and XRD for sol precursor. After the sol infiltration treatment, the coefficient of gas permeability dropped from 9.78×10-5 cm4·N-1·s-1 for as-deposited coating to 3.18×10-5 cm4·N-1·s-1 and 9.56×10-6 cm4·N-1·s-1 for coating after 4 and 8 times of infiltration treatment respectively. SEM analysis showed that the intergranular pores and gaps on the surface of as-deposited coating had been stuffed by the decomposed products from the sol. The coating surface became smoother and denser after densification treatment. A further SEM analysis of fracture surface of the infiltrated coating demonstrated that the sol had penetrated into the coating with depth of up to 3.5μm. The electrical conductivity in direction perpendicular to coating surface after 4 and 8 times of infiltration treatment increased no more than 10% comparable to that of as-deposited coating. Furthermore, an obvious increment in the electrical conductivities of electrolyte coatings between 4 and 8 times of infiltration treatment did not occurred. The electrical conductivity in direction perpendicular to coating surface after infiltration treatment was still lower than that of bulk 8YSZ by 30%.
According to the measurement results of output performances of unit cells at 800°C, an open circuit voltage (OCV) of 0.820V was obtained for the cell using as-deposited electrolyte coating. At the same time, the OCV increased to 1.017V and 1.036V for cells using electrolyte coatings after 4 and 8 times of infiltration treatments respectively. For the cell employing as-deposited coating as electrolyte, a maximum output powder density of 70mW/cm2 was obtained. On the contrary, the maximum output powder densities increased to 140mW/cm2 and 153mW/cm2 for cells using electrolyte coatings after 4 and 8 times of infiltration treatments respectively.
At the same time, Ni-YSZ coatings were prepared by EB-PVD through simultaneously evaporating two ingots of metal Ni and YSZ. SEM analysis demonstrated that these coating exhibited a typical columnar growth pattern. Between the loose columns, there were many gaps and pores. TEM analysis showed that many fine grains and nano-sized pores existed in this coating. According to N2 adsorption results, the surface specific area of this coating was up to 3.232m2/g. At the same time, the average pore diameter of 25nm and total pore volume of 0.0202cm3/g were obtained. Due to the strengthening effects of the addition of the second phase particles on coating porosity, the porosity of this coating increased from 12% to 19% when the Ni content in the coating increased from 18% to 44%. On the contrary, when the Ni content further increased to 63%, the coating porosity decreased from 19% to 11%. The electrical conductivity behavior of Ni-YSZ coating showed an S-shaped curve accompanying the increase of Ni content.
NiO-YSZ coatings were prepared by EB-PVD through simultaneously evaporating two ingots of NiO and YSZ and then the final Ni-YSZ coatings were obtained after a reduction treatment at 800oC in hydrogen for 2h. SEM analysis showed that the pore diameters were mainly in the range from tens of nanometers to hundreds of nanometers and the characteristics of columnar grains vanished. Comparable to the Ni-YSZ coatings prepared through directly evaporating two ingots of Ni and YSZ, the specific surface area increased from 3.232m2/g to 4.330m2/g for final Ni-YSZ coatings obtained from NiO-YSZ coatings a reduction treatment. At the same time, the total pore volume also increased from 0.02024cm3/g to 0.03460cm3/g. A graded coating, with gradient not only in element distribution but also in porosity distribution along the direction across coating thickness, was realized through adjusting and controlling the electron beam currents. In this graded coating, a high porosity and big pore diameter were achieved in one side closed to substrate, while a low porosity and small pore diameter were obtained in the other side close to coating surface. On the basis of anode preparations mentioned above, a continuous deposition of YSZ electrolyte coating was realized through shutting off electron beam current for evaporating NiO ingot, consequently resulting in a continuous deposition of anode and electrolyte coatings for SOFCs.
采用EB-PVD工艺在多孔的NiO-YSZ基体上制备了8YSZ电解质涂层,制备态及1000°C退火后的涂层均由单一的立方YSZ相组成。电解质涂层的SEM分析表明,涂层呈现出典型的柱状晶结构,在柱状晶间隙处存在微米级的孔隙。涂层元素沿断面分布的EPMA分析结果表明,涂层内的Zr、Y、O元素分布均匀。TEM分析结果表明,涂层的断面由条形或锥形的晶粒组成,在这些晶粒的内部呈现出许多宽度为几纳米并按照一定角度倾斜的白色迹线。
气密性测试结果表明,EB-PVD工艺制备的YSZ电解质涂层的气体扩散系数为9.78×10-5 cm4·N-1·s-1,此值较大气等离子喷涂制得的电解质涂层的气体扩散系数降低了60%以上。YSZ电解质涂层的电导率表现出显著的各向异性,在500°C~800°C的温度范围内,电解质涂层垂直于涂层表面方向的电导率均显著高于平行于表面方向的电导率。根据Arrhenius方程计算出的垂直于涂层表面方向和平行于涂层表面方向的电导活化能分别为80.884kJ/mol和110.147kJ/mol。采用低压浸渗装置对EB-PVD制备的电解质涂层进行了溶胶浸渗处理,根据对溶胶前驱体粉末进行的DSC-TG分析和XRD分析结果确定了致密化的烧结工艺。经过溶胶浸渗处理之后,电解质涂层的气体扩散系数从制备态的9.78×10-5 cm4·N-1·s-1下降至4次和8次溶胶浸渗处理后的3.18×10-5 cm4·N-1·s-1和9.56×10-6 cm4·N-1·s-1。SEM分析表明,溶胶浸渗处理之后,制备态电解质涂层表面晶体颗粒之间的孔隙和缺陷被溶胶所填充,涂层表面变得光滑、致密;断面分析表明,溶胶渗入涂层的深度可达3.5μm。相对于制备态涂层材料的电导率,经过4次和8次溶胶浸渗处理之后,垂直于涂层表面方向电导率提高的幅度均在10%以内,且8次浸渗处理相对4次浸渗处理之后涂层电导率的提高不明显。溶胶浸渗处理后8YSZ电解质涂层垂直于涂层表面的电导率仍比块体材料电导率低30%左右。
单电池800°C的输出性能表明,采用制备态YSZ涂层作为电解质材料的单电池其开路电压为0.820V,采用经过4次和8次溶胶浸渗处理后的涂层作为电解质材料的单电池,其开路电压分别升高至1.017V和1.036V。对于采用制备态电解质涂层的单电池,其最大输出功率密度为70mW/cm2;电解质涂层经过4次和8次浸渗处理后,单电池的最大输出功率密度分别提高到为140mW/cm2和153 mW/cm2。
与此同时,采用双源蒸发工艺,通过同时蒸发金属Ni和YSZ锭料沉积制备了Ni-YSZ涂层。SEM分析表明,Ni-YSZ涂层表现为典型的柱状晶生长模式。TEM分析表明涂层内的晶粒细小且含有大量纳米级的孔隙。N2吸附曲线结果表明,涂层的比表面积为3.232m2/g,平均孔径为25nm,总的孔体积为0.0202cm3/g。由于第二相粒子的加入对阴影效应的强化作用,当Ni含量由18%增加至44%时,Ni-YSZ涂层的孔隙率亦由12%增长至19%;当Ni含量进一步增长至63%,涂层的孔隙率呈现出下降趋势,由19%下降至11%。随着Ni含量的变化,Ni-YSZ涂层的电导率表现出了典型的S形曲线。
采用双源蒸发工艺,通过同时蒸发NiO和YSZ锭料沉积制备了NiO-YSZ涂层,并在800oC氢气气氛下还原2h得到最终的Ni-YSZ涂层。SEM分析表明涂层的孔隙直径大部分在几十纳米到几百纳米范围内。相对于直接利用EB-PVD工艺制备的Ni-YSZ涂层,NiO-YSZ涂层经过还原处理得到的Ni-YSZ涂层,其比表面积由3.232m2/g提高到4.330m2/g,总的孔隙体积由0.02024cm3/g提高到0.03460cm3/g。通过对电子束流的控制,成功制备出了一种成分及孔隙率均沿断面连续变化的梯度涂层,涂层在靠近基板一侧孔隙率及孔隙直径较大,而在靠近表面一侧涂层的孔隙直径以及孔隙率均明显变小。在采用上述方法制得NiO-YSZ阳极涂层的基础上,关闭用于蒸发NiO的电子束电流,通过连续沉积制备了YSZ电解质涂层,实现了SOFC阳极及电解质涂层的连续沉积。
Electron beam physical vapor deposition (EB-PVD) technique was employed to prepare the Ni-YSZ anode coatings as well as the YSZ electrolyte coatings for SOFCs in this study. The chemical composition and microstructure of the coatings were analyzed by x-ray fluorescence spectra (XRF), x-ray diffraction (XRD), scanning electron microscope (SEM), electron probe mciroanalysis (EPMA), transmitting electron microscope (TEM), and atom force microscope (AFM). Then the properties of these coatings, such as porosity, gas tightness, electrical conductivity and so on, were measured and characterized. At the same time, unit cells were assembled and output performances were investigated.
8YSZ electrolyte coatings were prepared by EB-PVD process on porous NiO-YSZ substrates. Both the as-deposited coating and the coating annealed at 1000°C consisted of a single phase of cubic YSZ. SEM analysis demonstrated that electrolyte coating exhibited a characteristic columnar structure. In gaps between the columns, there were many pores with the magnitude of micrometers. A uniform distribution of zirconium, yttrium and oxygen was realized along the direction across coating thickness according to EPMA. TEM analysis indicated that there were many crystalline grains with shapes of strip and pyramid in coating cross-section. Many white lines, with the width of several nanometers, appeared within these grains and inclined with some angle.
Gas-tightness measurement results demonstrated that a gas permeability of 9.78×10-5 cm4·N-1·s-1 was obtained for YSZ electrolyte prepared by EB-PVD, which was lower than that of electrolyte coating prepared by atmosphere plasma spraying by 60%. The electrical conductivity of YSZ electrolyte coating exhibited a typical anisotropy. In temperature range of 500°C~800°C, the electrical conductivity in direction perpendicular to coating surface was obviously higher that in direction parallel to coating surface. According to Arrhenius equation, activation energies for electrical conduction in the directions both perpendicular and parallel to coating surface were 80.884kJ/mol and 110.147kJ/mol respectively.
A sol infiltration device at subatmospheric pressure was used to densify the YSZ electrolyte coatings. Then the post-sintering process was determined according to the analysis results of DSC-TG and XRD for sol precursor. After the sol infiltration treatment, the coefficient of gas permeability dropped from 9.78×10-5 cm4·N-1·s-1 for as-deposited coating to 3.18×10-5 cm4·N-1·s-1 and 9.56×10-6 cm4·N-1·s-1 for coating after 4 and 8 times of infiltration treatment respectively. SEM analysis showed that the intergranular pores and gaps on the surface of as-deposited coating had been stuffed by the decomposed products from the sol. The coating surface became smoother and denser after densification treatment. A further SEM analysis of fracture surface of the infiltrated coating demonstrated that the sol had penetrated into the coating with depth of up to 3.5μm. The electrical conductivity in direction perpendicular to coating surface after 4 and 8 times of infiltration treatment increased no more than 10% comparable to that of as-deposited coating. Furthermore, an obvious increment in the electrical conductivities of electrolyte coatings between 4 and 8 times of infiltration treatment did not occurred. The electrical conductivity in direction perpendicular to coating surface after infiltration treatment was still lower than that of bulk 8YSZ by 30%.
According to the measurement results of output performances of unit cells at 800°C, an open circuit voltage (OCV) of 0.820V was obtained for the cell using as-deposited electrolyte coating. At the same time, the OCV increased to 1.017V and 1.036V for cells using electrolyte coatings after 4 and 8 times of infiltration treatments respectively. For the cell employing as-deposited coating as electrolyte, a maximum output powder density of 70mW/cm2 was obtained. On the contrary, the maximum output powder densities increased to 140mW/cm2 and 153mW/cm2 for cells using electrolyte coatings after 4 and 8 times of infiltration treatments respectively.
At the same time, Ni-YSZ coatings were prepared by EB-PVD through simultaneously evaporating two ingots of metal Ni and YSZ. SEM analysis demonstrated that these coating exhibited a typical columnar growth pattern. Between the loose columns, there were many gaps and pores. TEM analysis showed that many fine grains and nano-sized pores existed in this coating. According to N2 adsorption results, the surface specific area of this coating was up to 3.232m2/g. At the same time, the average pore diameter of 25nm and total pore volume of 0.0202cm3/g were obtained. Due to the strengthening effects of the addition of the second phase particles on coating porosity, the porosity of this coating increased from 12% to 19% when the Ni content in the coating increased from 18% to 44%. On the contrary, when the Ni content further increased to 63%, the coating porosity decreased from 19% to 11%. The electrical conductivity behavior of Ni-YSZ coating showed an S-shaped curve accompanying the increase of Ni content.
NiO-YSZ coatings were prepared by EB-PVD through simultaneously evaporating two ingots of NiO and YSZ and then the final Ni-YSZ coatings were obtained after a reduction treatment at 800oC in hydrogen for 2h. SEM analysis showed that the pore diameters were mainly in the range from tens of nanometers to hundreds of nanometers and the characteristics of columnar grains vanished. Comparable to the Ni-YSZ coatings prepared through directly evaporating two ingots of Ni and YSZ, the specific surface area increased from 3.232m2/g to 4.330m2/g for final Ni-YSZ coatings obtained from NiO-YSZ coatings a reduction treatment. At the same time, the total pore volume also increased from 0.02024cm3/g to 0.03460cm3/g. A graded coating, with gradient not only in element distribution but also in porosity distribution along the direction across coating thickness, was realized through adjusting and controlling the electron beam currents. In this graded coating, a high porosity and big pore diameter were achieved in one side closed to substrate, while a low porosity and small pore diameter were obtained in the other side close to coating surface. On the basis of anode preparations mentioned above, a continuous deposition of YSZ electrolyte coating was realized through shutting off electron beam current for evaporating NiO ingot, consequently resulting in a continuous deposition of anode and electrolyte coatings for SOFCs.
引文
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