Room temperature oxidative intercalation with chalcogen hydrides: Two-step method for the formation of alkali-metal chalcogenide arrays within layered perovskites |
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| Authors: | K.G. Sanjaya Ranmohotti M. Dariush Montasserasadi Jonglak Choi Yuan Yao Debasish Mohanty Elisha A. Josepha Shiva Adireddy Gabriel Caruntu John B. Wiley |
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| Affiliation: | 1. Instytut Fizyki, Uniwersytet Kazimierza Wielkiego w Bydgoszczy (UKW), Powstańców Wielkopolskich, Bydgoszcz 85-822, Poland;2. Electronics Department, Lviv National University, 50 Dragomanov Street, Lviv 79005, Ukraine;3. Institute for Scintillation Materials of NAS of Ukraine (ISMA), Lenin Avenue, 60, Kharkov 61158, Ukraine;1. Department of Chemical Engineering, University of South Carolina, Columbia, SC 29208, United States;2. Department of Chemistry & Biochemistry, University of South Carolina, Columbia, SC 29208, United States;1. College of Materials and textile, Zhejiang Sci-Tech University, Hangzhou 310018, China;2. Key Laboratory of Advanced Textile Materials and Manufacturing Technology of Ministry of Education, Zhejiang Sci-Tech University, Hangzhou 310018, China;1. School of Engineering, Design and Built Environment, Western Sydney University, Locked Bag 1797, Penrith, NSW, 2751, Australia;2. Advanced Materials Characterisation Facility, Western Sydney University, Locked Bag 1797, Penrith, NSW, 2751, Australia;1. NPE-LACOM – Federal University of Paraíba, 58051-900 João Pessoa, PB, Brazil;2. Univ. Rennes, CNRS, ISCR – UMR 6226, ScanMat – UMS 2001, F-35000 Rennes, France;3. Modeling and Molecular Simulation Group, INCTMN-UNESP, São Paulo State University, Bauru, SP, Brazil;4. Chemistry Institute, Federal University of Rio Grande do Norte, 59078-970 Natal, RN, Brazil |
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| Abstract: | A two-step topochemical reaction strategy utilizing oxidative intercalation with gaseous chalcogen hydrides is presented. Initially, the Dion-Jacobson-type layered perovskite, RbLaNb2O7, is intercalated reductively with rubidium metal to make the Ruddlesden-Popper-type layered perovskite, Rb2LaNb2O7. This compound is then reacted at room-temperature with in situ generated H2S gas to create Rb S layers within the perovskite host. Rietveld refinement of X-ray powder diffraction data (tetragonal, a = 3.8998(2) Å, c = 15.256(1) Å; space group P4/mmm) shows the compound to be isostructural with (Rb2Cl)LaNb2O7 where the sulfide resides on a cubic interlayer site surrounded by rubidium ions. The mass increase seen on sulfur intercalation and the refined S site occupation factor (～0.8) of the product indicate a higher sulfur content than expected for S2? alone. This combined with the Raman studies, which show evidence for an HS stretch, indicate that a significant fraction of the intercalated sulfide exists as hydrogen sulfide ion. Intercalation reactions with H2Se(g) were also carried out and appear to produce an isostructural selenide compound. The utilization of such gaseous hydride reagents could significantly expand multistep topochemistry to a larger number of intercalants. |
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