Molten salt synthesis of a mixed-valent lanthanide(III/IV) oxychloride with an unprecedented Sillen X(2)(4) structure: Ce1.3Nd0.7O3Cl |
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Authors: | Vigier Jean-François Renard Catherine Henry Natacha Laplace Annabelle Abraham Francis |
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Institution: | Unité de Catalyse et de Chimie du Solide, UCCS UMR CNRS 8181, ENSCL-USTL, Université Lille Nord de France, B.P. 90108, 59652 Villeneuve d'Ascq Cedex, France. |
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Abstract: | A new cerium neodymium oxychloride, Ce1.3Nd0.7O3Cl, has been synthesized by precipitation in a LiCl–CaCl2 molten salt by humid argon sparging. Chemical and structure characterization have been undertaken by powder X-ray diffraction, scanning electron microscopy, high-temperature X-ray diffraction, thermogravimetric analysis, and X-ray photoelectron scattering. This oxychloride crystallizes in space group P4/nmm, a = 3.9848(3) ? and c = 12.467(2) ?, in a new Sillen-type phase represented by the symbol X(2)(4) where “quadruple” fluorite-type layers M4O6], containing Ce(IV) in “inner” sublayers and both CeIII and NdIII in “outer” sublayers, alternate with double-halide ion sheets. The structure is also described as a stacking of LnOCl and fluorite-type blocks and constitutes the term n = 2 of a possible series (MO2)n(NdOCl)2. |
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