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Flux crystal growth of uranium(v) containing oxyfluoride perovskites

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Abstract

The novel phases Rb4NaU3O12−xFx (1), K4NaU3O12−xFx (2), and Rb2.1K1.9KU3O12−xFx (3) were synthesized by molten flux methods using mixed alkali fluoride melts. The oxyfluorides crystallize in the cubic space group Im[3 with combining macron]m with a lattice parameters of 8.7472(2) Å, 8.6264(2) Å, and 8.8390(3) Å, respectively. All three structures crystallize in a cubic perovskite structure, ABO3 (A4BB′3O12), where the A site is fully occupied by an alkali cation, and the B site is shared by the remaining smaller alkali cation and uranium in an ordered fashion such that the alkali cation on the B site is surrounded by square uranyl bipyramids. The structures were characterized by single crystal X-ray diffraction, energy dispersive spectroscopy, X-ray absorption near edge structure spectroscopy, X-ray photoelectron spectroscopy, magnetic susceptibility measurements, DFT calculations, thermogravimetric analysis, and UV-vis spectroscopy, all of which support the presence of U(V) in the three new materials.

Graphical abstract: Flux crystal growth of uranium(v) containing oxyfluoride perovskites

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Publication details

The article was received on 10 May 2019, accepted on 14 Sep 2019 and first published on 16 Sep 2019


Article type: Research Article
DOI: 10.1039/C9QI00537D
Inorg. Chem. Front., 2019, Advance Article

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    Flux crystal growth of uranium(V) containing oxyfluoride perovskites

    C. A. Juillerat, V. Kocevski, G. Morrison, S. G. Karakalos, D. Patil, S. T. Misture, T. M. Besmann and H. zur Loye, Inorg. Chem. Front., 2019, Advance Article , DOI: 10.1039/C9QI00537D

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