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Study of Crystallite Size of Yttria-Stabilized Zirconia powders by Rietveld Method

机译:Rietveld法研究氧化钇稳定的氧化锆粉末的微晶尺寸

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The yttria-stabilized zirconia (YSZ) is used in a great variety of applications, for example, electrolytes of solid oxide fuel cells and oxygen sensors. In the study of YSZ, the particle size powders and sintering processes are important to define the final properties of the zirconia products. The objectives of this work were to determine the phases and the crystalline size using X-Ray Diffraction (XRD) data and the Rietveld Method (RM) of the YSZ powders obtained by chemical synthesis based on the Pechini method. It was used Z1OCl_(2.8)H_2O and Y(NO_3)_(3.5)H_2O as precursors reagents. After calcination at 550°C during 24 hours, the powder was analyzed by XRD and scanning electronic microscopy (SEM). From XRD and using Rietveld method were verified that there is only cubic phase with lattice parameter a = 5.1307(1) A and the space group Fm3m. Due to substitution of the Zr atoms in the Y atoms sites, there were vacancies in 17.72 % of O atoms sites. However, the percentage of substitution of Zr atoms in Y atoms sites in the structure not was determinate because the curves of atomic scattering of them are very similar. Using Scherrer equation and considering anisotropy effect, the average crystalline size was determinate: 10,43 nm (c axis) and 10,39 (b axis). This spherical symmetry also observed for SEM.
机译:氧化钇稳定的氧化锆(YSZ)用于多种应用,例如,固体氧化物燃料电池的电解质和氧传感器。在YSZ的研究中,粒度粉末和烧结工艺对于确定氧化锆产品的最终性能很重要。这项工作的目的是使用X射线衍射(XRD)数据和RiPeveld方法(RM)确定通过Pechini方法化学合成获得的YSZ粉末的相和晶体尺寸。使用Z1OCl_(2.8)H_2O和Y(NO_3)_(3.5)H_2O作为前体试剂。在550℃下煅烧24小时后,通过XRD和扫描电子显微镜(SEM)分析粉末。通过XRD和Rietveld方法验证了只有晶格参数a = 5.1307(1)A的立方相和空间群Fm3m。由于在Y原子位点中Zr原子的取代,在O原子位点中有17.72%的空位。然而,由于它们的原子散射曲线非常相似,因此无法确定结构中Y原子位点中Zr原子的取代百分比。使用Scherrer方程并考虑各向异性效应,确定平均晶体尺寸:10.43 nm(c轴)和10.39 nm(b轴)。对于SEM也观察到这种球形对称性。

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