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Quantification of Cr in Lu1-xSrxFe0.5Cr0.5O3 (0 ≤ x ≤ 1) samples containing impurities using X-ray techniques in combination with several data treatment methodologies
Journal of Physics and Chemistry of Solids ( IF 4 ) Pub Date : 2021-06-02 , DOI: 10.1016/j.jpcs.2021.110200
Florencia E. Lurgo , Silvina Limandri , Raúl E. Carbonio , Germán Tirao

Wet chemical method was applied with the intention of obtaining Lu1-xSrxFe0.5Cr0.5O3 (0 ≤ x ≤ 1) perovskites in polycrystalline form. A systematic study of the crystal structure of the main perovskite phase obtained as well as a characterization of impurities was performed by X-ray techniques: powder diffraction (PXRD), high resolution emission spectroscopy (HR-XES), and photoelectron spectrometry (XPS). The PXRD data of Lu1-xSrxFe0.5Cr0.5O3 (0 ≤ x ≤ 1) were refined using Pbnm orthorhombic unit cell for the perovskite structure. Only samples with x = 0 and x = 0.1 resulted pure; as the amount of Sr increases, it is segregated as impurities, first as SrCrO4 and then as SrFe12O19. The mean oxidation state of Cr in the analyzed samples was obtained from HR-XES by quantifying spectral changes in the Cr-Kβ" and Cr-Kβ2,5 regions by different methodologies: statistical parameters and multivariate methods. The results were compared with the ones obtained by PXRD and XPS. With the last technique Cr6+ ionic concentrations were obtained through the spectral analysis in the region Cr2p3/2–580eV. Similar Cr6+ ionic compositions were obtained using the three X-ray techniques.



中文翻译:

使用 X 射线技术结合多种数据处理方法对含有杂质的Lu 1-x Sr x Fe 0.5 Cr 0.5 O 3 (0 ≤ x ≤ 1) 样品中的 Cr 进行定量

应用湿化学方法的目的是获得多晶形式的Lu 1-x Sr x Fe 0.5 Cr 0.5 O 3 (0 ≤ x ≤ 1) 钙钛矿。通过 X 射线技术对获得的主要钙钛矿相的晶体结构和杂质进行了系统研究:粉末衍射 (PXRD)、高分辨率发射光谱 (HR-XES) 和光电子能谱 (XPS) . Lu 1-x Sr x Fe 0.5 Cr 0.5 O 3的PXRD数据(0 ≤ x ≤ 1) 使用 Pbnm 正交晶胞对钙钛矿结构进行细化。只有 x = 0 和 x = 0.1 的样品才是纯的;随着Sr量的增加,它作为杂质分离,首先分离为SrCrO 4,然后分离为SrFe 12 O 19。分析样品中 Cr 的平均氧化态是通过 HR-XES通过不同方法(统计参数和多变量方法)量化 Cr-Kβ" 和 Cr-Kβ 2,5区域的光谱变化而获得的。结果与通过 PXRD 和 XPS 获得的。使用最后一种技术,通过光谱分析在 Cr2p 3/2 –580eV区域获得Cr 6+离子浓度。类似的 Cr 6+ 离子组合物是使用三种 X 射线技术获得的。

更新日期:2021-06-09
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