Discrepancy in the quantitative oxidation-state analysis of Eu species in sulfide phosphors by K-, L1- and L3-edge XANES spectrometry: choice of absorption edge and measurement mode,Journal of Analytical Atomic Spectrometry

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Discrepancy in the quantitative oxidation-state analysis of Eu species in sulfide phosphors by K-, L1- and L3-edge XANES spectrometry: choice of absorption edge and measurement mode
Journal of Analytical Atomic Spectrometry ( IF 3.1 ) Pub Date : 2018-02-23 00:00:00 , DOI: 10.1039/c7ja00429j
Takashi Yamamoto _{1,

2,

3,

4,

5} , Akira Yukumoto _{5,

6,

7,

8,

9}

Affiliation

A quantitative analysis of the oxidation state of europium (Eu) in phosphor samples was performed using X-ray absorption near-edge structure (XANES) spectrometry to investigate the influence of the constituent elements, absorption edge and measurement mode on the evaluated oxidation states. XANES spectra of two kinds of phosphor samples were recorded in fluorescence mode with a Lytle detector at the L1- and L3-edges and in transmission mode at the K-edge. The Eu species in the analysed samples were confirmed to be almost exclusively Eu²⁺via Eu K- and L1-edge XANES characterization, whereas L3-edge experiments exhibited the presence of Eu³⁺ up to a content of 35%. In cases wherein the absorption coefficients of constituent elements were higher than the penetration capability of fluorescence X-rays for detection, the quantitative oxidation-state analysis via L3- and L1-edge XANES analysis in fluorescence mode exhibited inconsistent results because of the differences in self-absorption for each emission line. An apparent chemical shift at Eu K-edge was found to be 7.5 ± 0.7 eV, which could provide a more accurate quantitative oxidation-state analysis of a bulk phase because of the large natural width for the K-shell and the penetration capability of an incident X-ray.

中文翻译：

K-，L1-和L3-edge XANES光谱法对硫化物荧光粉中Eu物种的定量氧化态分析的差异：吸收边缘和测量模式的选择

使用X射线吸收近边缘结构（XANES）光谱对荧光粉样品中of（Eu）的氧化态进行了定量分析，以研究组成元素，吸收边缘和测量模式对评估的氧化态的影响。两种荧光粉样品的XANES光谱在L1和L3边缘使用Lytle检测器以荧光模式记录，在K边缘以透射模式记录。通过Eu K-和L1边缘XANES表征，确认分析样品中的Eu种类几乎全部为Eu ²⁺，而L3边缘实验显示存在Eu ³⁺含量最高可达35％。在组成元素的吸收系数高于荧光X射线的检测能力的情况下，由于自身差异，通过L3-和L1-edge XANES分析在荧光模式下进行的定量氧化态分析结果不一致。 -每个发射线的吸收。发现在Eu K边缘的表观化学位移为7.5±0.7 eV，由于K壳的自然宽度大且对K-壳的渗透能力强，因此可以提供对主体相更准确的定量氧化态分析。入射X射线。

更新日期：2018-02-23

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