Chemical Analysis of CsPbBr2X (X = Cl, I) Nanocomposites by Total Reflection X-Ray Fluorescence Spectroscopy (TXRF)

IF 0.9 4区材料科学 Q4 MATERIALS SCIENCE, MULTIDISCIPLINARY

Inorganic Materials Pub Date : 2024-03-20 DOI:10.1134/S0020168523140054

D. G. Filatova, A. S. Chizhov, M. N. Rumyantseva

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Abstract

An approach to TXRF determination of the composition of perovskite nanocomposites of the putative compositions CsPbBr₂Cl and CsPbBr₂I is proposed. Sample preparation consists in the treatment of hydrophobic samples with dimethylformamide (DMFA) and the subsequent dilution of the obtained solutions with water. When using a copper solution as an internal standard, the reproducibility of the results of TXRF determination of the elements is attained with S_r no more than 0.05. The validity of the determination of Cs, Pb, Br, and I is confirmed by the results of their determination by ICP-MS in solutions after processing samples in DMFA followed by dilution with 2% HNO₃ for Cs, Pb, and Br or tetramethylammonium hydroxide (TMAH) for Cs, Pb, Br, and I, whereas the determination of chlorides is confirmed by the method of direct potentiometry in diluted solutions. It is shown that lead does not form insoluble chlorides in the TMAH solution and does not interfere with the determination. The effect of bromides on the determination of chlorides is characterized by a potentiometric coefficient of 10^–3. The results obtained provide the determination of the stoichiometry of the synthesized compounds CsPbBr₂Cl and CsPbBr_2.7I_0.3.

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利用全反射 X 射线荧光光谱 (TXRF) 分析 CsPbBr2X（X = Cl，I）纳米复合材料的化学性质

摘要提出了一种利用 TXRF 测定推定成分 CsPbBr2Cl 和 CsPbBr2I 的包晶纳米复合材料成分的方法。样品制备包括用二甲基甲酰胺 (DMFA) 处理疏水性样品，然后用水稀释得到的溶液。使用铜溶液作为内标时，TXRF 元素测定结果的重现性不超过 0.05。在 DMFA 中处理样品后，用 2% HNO3 稀释 Cs、Pb、Br 和 I，或用四甲基氢氧化铵（TMAH）稀释 Cs、Pb、Br 和 I，然后用 ICP-MS 测定溶液中的 Cs、Pb、Br 和 I，其结果证实了测定 Cs、Pb、Br 和 I 的有效性。结果表明，铅在 TMAH 溶液中不会形成不溶性的氯化物，也不会干扰测定。溴化物对氯化物测定的影响以 10-3 的电位系数为特征。所获得的结果有助于确定合成化合物 CsPbBr2Cl 和 CsPbBr2.7I0.3 的化学计量学。

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来源期刊

Inorganic Materials 工程技术-材料科学：综合

CiteScore

1.40

自引率

25.00%

发文量

审稿时长

3-6 weeks

期刊介绍： Inorganic Materials is a journal that publishes reviews and original articles devoted to chemistry, physics, and applications of various inorganic materials including high-purity substances and materials. The journal discusses phase equilibria, including P–T–X diagrams, and the fundamentals of inorganic materials science, which determines preparatory conditions for compounds of various compositions with specified deviations from stoichiometry. Inorganic Materials is a multidisciplinary journal covering all classes of inorganic materials. The journal welcomes manuscripts from all countries in the English or Russian language.