Study on co-sintering characteristics of metal supported solid oxide fuel cells
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摘要: 在考虑电池整体热膨胀及陶瓷蠕变的情况下分析电极层和电解质层的烧结机理，阐明金属支撑固体氧化物燃料电池(MS-SOFC)在不同烧结温度及晶粒尺寸下电极和电解质层微观结构的演变、残余应力的分布及变化规律。通过建立Skorohod-Olevsky Viscous Sintering (SOVS)模型，模拟在不同烧结温度和不同晶粒尺寸下，MS-SOFC的各层和各界面的相对密度、应力的分布和演化，并通过高温烧结实验揭示异种晶粒尺寸结构烧结后微观结构形貌的变化。结果表明，电解质和电极的相对密度、各层的残余应力值和突变幅度受到烧结温度的影响。当燃料电池各层材料初始晶粒尺寸较小时，烧结导致的致密化率非常明显，随着晶粒尺寸逐渐增大，其致密化率相对较小，且电池各层的残余应力值和突变幅度逐渐减小。纳米氧化钇稳定氧化锆(YSZ)电解质层更容易烧结，且比亚微米YSZ电解质层烧结后微观缺陷降低更多。MS-SOFC烧结后，阴极和阳极的径向应力为拉伸应力，电解质的径向应力为压缩应力。轴向应力和剪切应力在拉压应力之间周期性变化。拥有微米晶的电极层能够在烧结后保持较大的孔隙率，而拥有纳米晶的电解质在提高电导率的同时还能够降低其致密化烧结温度。当晶体尺寸为纳米级时，残余应力值和分布对烧结温度很敏感。Abstract: The sintering mechanism of electrode layer and electrolyte layer was analyzed considering the whole thermal expansion of the battery and the creep of the ceramic. The evolution of the microstructure of the electrode and electrolyte layer and the distribution and change of residual stress of the metal supported solid oxide fuel cell (MS-SOFC) under different sintering temperature and grain size were expounded. The Skorohod-Olevsky Viscous Sintering (SOVS) model was established to simulate the relative density and stress distribution and evolution of different layers and different surfaces of MS-SOFC under different sintering temperatures and different grain sizes. The change of microstructure morphology of dissimilar grain size structure after sintering was revealed by high temperature sintering experiment. The results show that the relative density of electrolyte and electrode, the residual stress value of each layer and the mutation amplitude are affected by sintering temperature. When the initial grain size of each layer of fuel cell material is small, the densification rate caused by sintering is very obvious. With the gradual increase of grain size, the densification rate is relatively small, and the residual stress value and mutation amplitude of each layer of the battery are gradually reduced. Nano-yttrium oxide stabilized zirconia (YSZ) electrolyte layer is easier to sintering, and the micro-defects are reduced more than the micron YSZ electrolyte layer after sintering. After sintering of MS-SOFC, the radial stress of cathode and anode is tensile stress, and the radial stress of electrolyte is compressive stress. Axial stress and shear stress vary periodically between tensile and compressive stress. The electrode layer with micron crystals can maintain large porosity after sintering, while the electrolyte with nanocrystalline can improve the conductivity and reduce the densification sintering temperature. When the crystal size is nanometer, the residual stress value and distribution are sensitive to the sintering temperature.
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Key words:
- MS-SOFC /
- co-sintering /
- residual stress /
- sintering temperature /
- grain size
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图 4 热膨胀系数曲线 (a) 阴极(LSCF), (b) 电解质(YSZ), (c) 阳极(Nio-YSZ), (d) 金属支撑(Crofer 22 APU)
Figure 4. Coefficient of thermal expansion profile：(a) cathode(LSCF), (b) electrolyte(YSZ), (c) anode(Nio-YSZ), (d) metal matrix (Crofer 22 APU)
图 5 YSZ电解质粉末的微观形貌 (a) YSZ粉末的整体微观形貌，(b) YSZ单个颗粒的微观形貌
Figure 5. Microstructure of YSZ: (a) The overall micromorphology of YSZ powder, (b) Microscopic morphology of individual YSZ particles
图 6 不同烧结温度(a)阴极，(b)电解质，(c)阳极和不同晶粒尺寸(d)阴极，(e)电解质，(f)阳极下的相对密度变化趋势
Figure 6. The trend of relative density variation at different sintering temperatures: (a) Cathode, (b) Electrolyte, (c) Anode; Trends in relative density changes under different grain sizes: (d) Cathode, (e) Electrolyte, (f) Anode
图 7 电解质涂层
1250 ℃烧结前后SEM电镜图 (a)烧结前微米涂层，(b)烧结后裂纹区域，(c)烧结后截面形貌，(d)烧结前纳米涂层，(e)烧结后未熔化区域，(f)烧结后截面形貌，(g)涂层孔隙率和未熔化颗粒含量随烧结时间的示意图Figure 7. Electrolyte coatings prepared by supersonic plasma spraying and SEM electron micrographs before and after sintering at
1250 ℃：(a) Micron coating before sintering，(b) Cracked area after sintering，(c) Cross-sectional morphology after sintering，(d) Nanocoatings before sintering，(e) Unmelted area after sintering，(f) Cross-sectional morphology after sintering，(g) Schematic diagram of coating porosity and unfused particle content with sintering time
图 8 各层晶粒尺寸优化后不同烧结温度下的相对密度变化趋势 (a)阴极，(b)电解质，(c)阳极
Figure 8. Trend of relative density changes at different sintering temperatures after optimizing the grain size of each layer：(a) Cathode, (b) Electrolyte, (c) Anode
图 9 微米涂层与纳米涂层
1250 ℃烧结后的透射电镜(TEM)图 (a)烧结后晶粒尺寸在200-600 nm之间的微米涂层的TEM图像，(b)烧结后晶粒尺寸在200- 500 nm之间的纳米涂层的TEM图像，(c)烧结后晶粒尺寸在20-90 nm之间的纳米涂层的TEM图像，(d)纳米涂层烧结后未熔化颗粒的晶粒尺寸在30-50 nm之间Figure 9. Transmission electron microscopy (TEM) of micron coating and nano coating after sintering at
1250 ℃：(a) TEM image of the sintered micron coating with grain size between 200-600 nm, (b) TEM image of the sintered nano-coating with grain size between 200-500 nm, (c) TEM image of the sintered nano-coating with grain size between 20-90 nm,(d) The unmelted particles after sintering of the nano-coating have a grain size between 30-50 nm
图 10 MS-SOFC的径向残余应力S11分布 (a)- (c)晶粒尺寸为30 nm时应力S11随温度的分布，(d)- (f)晶粒尺寸为500 nm时应力S11随温度的分布，(g)- (i)晶粒尺寸为
1300 nm时应力S11随温度的分布Figure 10. Radial residual stress S11 distribution of MS-SOFC：(a)- (c) Stress S11 distribution with temperature for grain size of 30 nm，(d)- (f) Stress S11 distribution with temperature for grain size of 500 nm，(g)- (i) Stress S11 distribution with temperature for grain size of
1300 nm
图 11 不同烧结温度下的径向残余应力S11分布 (a)阴极-30 nm，(b)电解质-30 nm，(c)阳极-30 nm，(d)阳极(无金属基体)-30 nm，(e)阳极-500 nm和
1300 nmFigure 11. The radial residual stress S11 distribution with different sintering temperatures：(a) cathode-30 nm，(b) electrolyte-30 nm，(c) anode-30 nm，(d) anode (Without metal matrix)-30 nm，(e) anode-500 nm&
1300 nm
图 12 不同晶体尺寸的径向残余应力S11分布 (a)阴极，(b)电解质，(c)阳极Fig.12 The radial residual stress S11 distribution with different crystal sizes：(a) cathode, (b) electrolyte, (c) anode
图 13 MS-SOFC的轴向残余应力S22分布 (a)- (c)晶粒尺寸为30 nm时应力S22随温度的分布，(d)- (f)晶粒尺寸为500 nm时应力S22随温度的分布，(g)- (i)晶粒尺寸为
1300 nm时应力S22随温度的分布Figure 13. Axial residual stress S22 distribution of MS-SOFC：(a)- (c) Stress S22 distribution with temperature for grain size of 30 nm，(d)- (f) Stress S22 distribution with temperature for grain size of 500 nm，(g)- (i) Stress S22 distribution with temperature for grain size of
1300 nm
图 14 不同烧结温度(a)阴极，(b)电解质，(c)阳极和不同晶粒尺寸(d)阴极，(e)电解质，(f)阳极下的轴向残余应力S22分布
Figure 14. The axial residual stress S22 distribution with different sintering temperatures：(a) cathode, (b) electrolyte, (c) anode；The axial residual stress S22 distribution with different crystal sizes：(d) cathode, (e) electrolyte, (f) anode
图 15 MS-SOFC的剪切残余应力S12分布 (a)- (c)晶粒尺寸为30 nm时应力S12随温度的分布，(d)- (f)晶粒尺寸为500 nm时应力S12随温度的分布，(g)- (i)晶粒尺寸为
1300 nm时应力S12随温度的分布Figure 15. Shear residual stress S12 distribution of MS-SOFC：(a)- (c) Stress S12 distribution with temperature for grain size of 30 nm，(d)- (f) Stress S12 distribution with temperature for grain size of 500 nm，(g)- (i) Stress S12 distribution with temperature for grain size of
1300 nm
图 16 不同烧结温度(a)阴极，(b)电解质，(c)阳极和不同晶粒尺寸(d)阴极，(e)电解质，(f)阳极下的剪切残余应力S12分布
Figure 16. The shear residual stress S12 distribution with different sintering temperatures：(a) cathode, (b) electrolyte, (c) anode; The shear residual stress S12 distribution with different crystal sizes：(d) cathode, (e) electrolyte, (f) anode
图 17 晶粒尺寸优化前后残余应力随表面温度变化的趋势 (a) s11阴极，(b) s11电解质，(c) s11阳极，(d) s22阴极，(e) s22电解质，(f) s22阳极，(g) s12阴极，(h) s12电解质，(i) s12阳极
Figure 17. Trend of residual stress with surface temperature before and after grain size optimization：(a) S11-cathode, (b) S11-electrolyte, (c) S11-anode,(d) S22-cathode, (e) S22-electrolyte, (f) S22-anode, (g) S12-cathode, (h) S12-electrolyte, (i) S12-anode
表 1 有限元分析中使用的材料特性
Table 1. Materials properties used in finite element analysis
Material properties Cathode (LSCF) Electrolyte (YSZ) Anode (NiO-YSZ) Metal matrix (Crofer 22 APU) Elasticity modulus/GPa 41.30 196.30 126.50 140 Poisson ratio 0.33 0.32 0.31 0.30 Thermal conductivity/(W·(m·℃)−1) 7.20 1.50 4.70 19.40 Specific heat/(J·(kg·℃)−1) 577 500 595 487 Density/(kg·m−3) 6070 206870 5280 7670 Notes：Lanthanum Strontium Cobalt Ferrite (LSCF) is a perovskite type oxide; YSZ is yttrium stabilized zirconia; NiO-YSZ is a mixture of nickel oxide and yttrium stabilized zirconia powder; Crofer 22 APU is a ferritic high temperature stainless steel. 
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表 2 电极和电解质层的蠕变参数
Table 2. Creep parameters of electrode and electrolyte layer
Parameter name Cathode (LSCF) Electrolyte (YSZ) Anode (NiO-YSZ) Viscosity parameters $ {\mu }_{0}/( $Pa·s) 6.0×1010 5.8×1010 6.2×1010 Creep temperature $ {T}_{t}/ $℃ 1150 1160 1040 Activation energy of viscous flow $ {Q}_{\mathrm{V}}/ $(kJ·mol−1) 27.85×103 25.0×103 20.0×103 Surface energy $ {\gamma }_{\mathrm{S}\mathrm{V}} $/(J·m−2) 1.80 1.27 1.50
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表 3 半电池样品的YSZ电解质喷涂工艺参数
Table 3. YSZ electrolyte spraying process parameters of half battery sample
Current/
AVoltage/
VHydrogen flow
rate/slpmArgon flow
rate/slpmSpray
distance/mm540 100 15 80 100
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