{"title":"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","authors":"D. G. Filatova, A. S. Chizhov, M. N. Rumyantseva","doi":"10.1134/S0020168523140054","DOIUrl":null,"url":null,"abstract":"<p>An approach to TXRF determination of the composition of perovskite nanocomposites of the putative compositions CsPbBr<sub>2</sub>Cl and CsPbBr<sub>2</sub>I 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 <i>S</i><sub><i>r</i></sub> 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% HNO<sub>3</sub> 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<sup>–3</sup>. The results obtained provide the determination of the stoichiometry of the synthesized compounds CsPbBr<sub>2</sub>Cl and CsPbBr<sub>2.7</sub>I<sub>0.3</sub>.</p>","PeriodicalId":585,"journal":{"name":"Inorganic Materials","volume":"59 14","pages":"1414 - 1417"},"PeriodicalIF":0.9000,"publicationDate":"2024-03-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":"{\"title\":\"Chemical Analysis of CsPbBr2X (X = Cl, I) Nanocomposites by Total Reflection X-Ray Fluorescence Spectroscopy (TXRF)\",\"authors\":\"D. G. Filatova, A. S. Chizhov, M. N. Rumyantseva\",\"doi\":\"10.1134/S0020168523140054\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"<p>An approach to TXRF determination of the composition of perovskite nanocomposites of the putative compositions CsPbBr<sub>2</sub>Cl and CsPbBr<sub>2</sub>I 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 <i>S</i><sub><i>r</i></sub> 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% HNO<sub>3</sub> 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<sup>–3</sup>. The results obtained provide the determination of the stoichiometry of the synthesized compounds CsPbBr<sub>2</sub>Cl and CsPbBr<sub>2.7</sub>I<sub>0.3</sub>.</p>\",\"PeriodicalId\":585,\"journal\":{\"name\":\"Inorganic Materials\",\"volume\":\"59 14\",\"pages\":\"1414 - 1417\"},\"PeriodicalIF\":0.9000,\"publicationDate\":\"2024-03-20\",\"publicationTypes\":\"Journal Article\",\"fieldsOfStudy\":null,\"isOpenAccess\":false,\"openAccessPdf\":\"\",\"citationCount\":\"0\",\"resultStr\":null,\"platform\":\"Semanticscholar\",\"paperid\":null,\"PeriodicalName\":\"Inorganic Materials\",\"FirstCategoryId\":\"88\",\"ListUrlMain\":\"https://link.springer.com/article/10.1134/S0020168523140054\",\"RegionNum\":4,\"RegionCategory\":\"材料科学\",\"ArticlePicture\":[],\"TitleCN\":null,\"AbstractTextCN\":null,\"PMCID\":null,\"EPubDate\":\"\",\"PubModel\":\"\",\"JCR\":\"Q4\",\"JCRName\":\"MATERIALS SCIENCE, MULTIDISCIPLINARY\",\"Score\":null,\"Total\":0}","platform":"Semanticscholar","paperid":null,"PeriodicalName":"Inorganic Materials","FirstCategoryId":"88","ListUrlMain":"https://link.springer.com/article/10.1134/S0020168523140054","RegionNum":4,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"Q4","JCRName":"MATERIALS SCIENCE, MULTIDISCIPLINARY","Score":null,"Total":0}
Chemical Analysis of CsPbBr2X (X = Cl, I) Nanocomposites by Total Reflection X-Ray Fluorescence Spectroscopy (TXRF)
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 Sr 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 CsPbBr2.7I0.3.
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.
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