Spatially resolved stoichiometry determination of Li7La3Zr2O12 solid-state electrolytes using LA-ICP-OES,Journal of Analytical Atomic Spectrometry

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Spatially resolved stoichiometry determination of Li7La3Zr2O12 solid-state electrolytes using LA-ICP-OES
Journal of Analytical Atomic Spectrometry ( IF 3.1 ) Pub Date : 2020-03-26 , DOI: 10.1039/d0ja00051e
Stefan Smetaczek _{1,

2,

3} , Maximilian Bonta _{1,

2,

3} , Andreas Wachter-Welzl _{1,

2,

3} , Stefanie Taibl _{1,

2,

3} , Reinhard Wagner _{3,

4,

5,

6} , Daniel Rettenwander _{3,

7,

8,

9} , Jürgen Fleig _{1,

2,

3} , Andreas Limbeck _{1,

2,

3}

Affiliation

Cubic Li₇La₃Zr₂O₁₂ (LLZO) garnets are among the most promising solid-state electrolytes for next-generation Li batteries. However, despite intensive research in recent years, little effort is spent on proper chemical analysis of the material. For reliable LLZO investigation, knowledge about the exact chemical composition, especially the Li content, is of uttermost importance. Herein, we present a method for the laterally resolved stoichiometry determination of Al stabilized LLZO (Li_7−3xAl_xLa₃Zr₂O₁₂) using LA-ICP-OES. To ensure reliable signal quantification, matrix-matched standards are prepared and carefully characterized using sample digestion and liquid ICP-OES measurement. An internal standard-independent calibration strategy based on 100 m% normalization is applied, enabling the quantification of all cations within the material. By comparing the obtained high-precision LA-ICP-OES calibrations with analog LA-ICP-MS measurements, it is shown that ICP-OES is the superior choice for the analysis of Li. The developed method is applied to record quantitative distribution images of an Al stabilized LLZO pellet, revealing macroscopic stoichiometry variations within the sample. To verify the analysis, the average stoichiometry obtained by the LA measurements is compared with the bulk composition determined via liquid ICP-OES analysis after sample fusion. The obtained values show excellent agreement, confirming the accuracy of the developed method.

中文翻译：

使用LA-ICP-OES的Li7La3Zr2O12固态电解质的空间分辨化学计量法

立方晶Li ₇ La ₃ Zr ₂ O ₁₂（LLZO）石榴石是下一代锂电池最有希望的固态电解质之一。然而，尽管近年来进行了深入的研究，但是很少花费精力来对材料进行适当的化学分析。为了进行可靠的LLZO研究，最重要的是要知道确切的化学组成，尤其是Li含量。在这里，我们提出一种横向稳定的化学计量测定铝稳定的LLZO（Li _{7-3 x} Al _x La ₃ Zr ₂ O ₁₂）使用LA-ICP-OES。为确保可靠的信号定量，需要准备基质匹配的标准液，并使用样品消解和液相ICP-OES测量对其进行仔细表征。采用基于100 m％归一化的独立于内部标准的校准策略，可对材料中的所有阳离子进行定量。通过将获得的高精度LA-ICP-OES校准值与模拟LA-ICP-MS测量值进行比较，可以看出ICP-OES是分析Li的最佳选择。所开发的方法用于记录Al稳定的LLZO颗粒的定量分布图像，揭示了样品中的宏观化学计量变化。为了验证分析结果，将通过LA测量获得的平均化学计量与通过样品融合后的液相ICP-OES分析。所获得的值显示出极好的一致性，证实了所开发方法的准确性。

更新日期：2020-03-26

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