All-Inorganic Open-Framework Chalcogenides, A3Ga5S9·xH2O (A = Rb and Cs), Exhibiting Ultrafast Uranyl Remediation and Illustrating a Novel Post-Synthetic Preparation of Open-Framework Oxychalcogenides

Berseneva, Anna A.; Aziziha, Mina; Schorne-Pinto, Juliano; Besmann, Theodore M.; zur Loye, Hans-Conrad

doi:10.1021/acs.chemmater.2c02059

Title: All-Inorganic Open-Framework Chalcogenides, A₃Ga₅S₉·xH₂O (A = Rb and Cs), Exhibiting Ultrafast Uranyl Remediation and Illustrating a Novel Post-Synthetic Preparation of Open-Framework Oxychalcogenides

Journal Article · Thu Sep 08 00:00:00 EDT 2022 · Chemistry of Materials

DOI:https://doi.org/10.1021/acs.chemmater.2c02059· OSTI ID:1905732

Berseneva, Anna A. ^[1];

^[1];

^[1]; Besmann, Theodore M. ^[1];

^[1]

Univ. of South Carolina, Columbia, SC (United States)

Fast and effective uranyl sequestration is of interest to the nuclear industry. Recently layered chalcogenide materials have demonstrated fast, selective, and efficient sorption properties towards uranyl cations and the development and investigation of new types of chalcogenide materials continues to be of interest and represents an intriguing option for uranyl remediation. Three new all-inorganic A₃Ga₅S₉·xH₂O (A = Rb, Rb/Cs, and Cs) open-framework chalcogenides were obtained via an in-situ alkali carbonate to alkali sulfide conversion process achieved under mild hydrothermal conditions. The structures of the all-inorganic open framework chalcogenides consist of a 2-fold interpenetrated diamond-like 3D framework containing pseudo-T₃ [Ga₁₀S₂₀]^10– supertetrahedra. 48% of the structural volume is occupied by A⁺ cations and water species, as established by single-crystal X-ray diffraction (SCXRD), infrared (IR) and energy-dispersive (EDS) spectroscopies. The dynamic nature of the A⁺ cations and water molecules within the pores was investigated via single crystal X-ray diffraction as well as by IR spectroscopy monitored H₂O to D₂O exchange experiments. Framework stability was probed with post-synthetic treatment of A₃Ga₅S₉·xH₂O (A = Rb and Cs) samples in acidic solutions that resulted in the formation of the oxysulfide (A/H)₃Ga₅S_9–yO_y·xH₂O (A = Rb and Cs; y = 0–1), as shown by SCXRD and IR. Ion-exchange studies on A₃Ga₅S₉·xH₂O (A = Rb and Cs) samples were carried out utilizing a uranyl acetate solution. The presence of the UO₂²⁺ species in the ion-exchanged product was supported by IR and EDS spectroscopies. Batch method ion-exchange experiments on Cs₃Ga₅S₉·xH₂O powder demonstrated fast kinetics with 95% uranyl removal from the uranyl acetate solution during the first minute, a maximum uranyl uptake capacity of 15mg/g, and the subsequent elution of uranyl species with KCl solution. Furthermore, the porous and dynamic nature of the A₃Ga₅S₉·xH₂O framework coupled with effective UO₂²⁺···S^2– bonding interactions makes it a good potential sorbent for uranyl remediation from aqueous media.

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Research Organization:: Univ. of South Carolina, Columbia, SC (United States)

Sponsoring Organization:: USDOE Office of Science (SC), Basic Energy Sciences (BES). Materials Sciences & Engineering Division

Grant/Contract Number:: SC0018739

OSTI ID:: 1905732

Journal Information:: Chemistry of Materials, Vol. 34, Issue 18; ISSN 0897-4756

Publisher:: American Chemical Society (ACS)Copyright Statement

Country of Publication:: United States

Language:: English

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37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY
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Chalcogenides
Chemical structure
Crystal structure
Uranium

Title: All-Inorganic Open-Framework Chalcogenides, A3Ga5S9·xH2O (A = Rb and Cs), Exhibiting Ultrafast Uranyl Remediation and Illustrating a Novel Post-Synthetic Preparation of Open-Framework Oxychalcogenides

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Title: All-Inorganic Open-Framework Chalcogenides, A₃Ga₅S₉·xH₂O (A = Rb and Cs), Exhibiting Ultrafast Uranyl Remediation and Illustrating a Novel Post-Synthetic Preparation of Open-Framework Oxychalcogenides