Synthesis and structure resolution of RbLaF4

Anne-Laure Rollet (1) , Mathieu Allix (2, 3) , Emmanuel Véron (2, 3) , Michael Deschamps (2, 3) , Valérie Montouillout (2, 3) , Matthew R. Suchomel (4) , Emmanuelle Suard (5) , Maud Barré (6) , Manuel Ocaña (7) , Aymeric Sadoc (8) , Florent Boucher (8) , Catherine Bessada (2, 3) , Dominique Massiot (2, 3) , Franck Fayon (2, 3)

1 PECSA - Physicochimie des Electrolytes, Colloïdes et Sciences Analytiques
2 CEMHTI - Conditions Extrêmes et Matériaux : Haute Température et Irradiation
3 UO - Université d'Orléans
4 ANL - Argonne National Laboratory [Lemont]
5 ILL - Institut Laue-Langevin
6 IMMM - Institut des Molécules et Matériaux du Mans
7 ICMSE - Instituto de Ciencia de Materiales de Sevilla
8 IMN - Institut des Matériaux Jean Rouxel

The synthesis and structure resolution of RbLaF4 are described. RbLaF4 is synthesized by solid-state reaction between RbF and LaF3 at 425 °C under a nonoxidizing atmosphere. Its crystal structure has been resolved by combining neutron and synchrotron powder diffraction data refinements (Pnma,a = 6.46281(2) Å, b = 3.86498(1) Å, c = 16.17629(4) Å, Z = 4). One-dimensional 87Rb, 139La, and 19F MAS NMR spectra have been recorded and are in agreement with the proposed structural model. Assignment of the 19F resonances is performed on the basis of both 19F–139La J-coupling multiplet patterns observed in a heteronuclear DQ-filtered J-resolved spectrum and 19F–87Rb HMQC MAS experiments. DFT calculations of both the 19F isotropic chemical shieldings and the 87Rb, 139La electric field gradient tensors using the GIPAW and PAW methods implemented in the CASTEP code are in good agreement with the experimental values and support the proposed structural model. Finally, the conductivity of RbLaF4 and luminescence properties of Eu-doped LaRbF4 are investigated.

Mots clés: Anions; Crystal structure; Magnetic properties; Nuclear magnetic resonance spectroscopy; Electrical conductivity

Domaines: Matériaux

Anne-Laure Rollet, Mathieu Allix, Emmanuel Véron, Michael Deschamps, Valérie Montouillout, et al.. Synthesis and structure resolution of RbLaF4. Inorganic Chemistry, 2012, 51, pp.2272. ⟨10.1021/ic202301e⟩. ⟨hal-00749155⟩