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Structural characterization of a new acentric protonated garnet: Li6−xHxCaLa2Nb2O12

Published online by Cambridge University Press:  27 August 2013

Cyrille Galven ,
Emmanuelle Suard ,
Denis Mounier ,
Marie-Pierre Crosnier-Lopez  and
Françoise Le Berre
Cyrille Galven
Affiliation:
LUNAM Université du Maine, Institut des Molécules et Matériaux du Mans (IMMM), 72085 Le Mans Cedex 9, France
Emmanuelle Suard
Affiliation:
Institut Laue-Langevin, 38042 Grenoble Cedex 9, France
Denis Mounier
Affiliation:
LUNAM Université du Maine, Institut des Molécules et Matériaux du Mans (IMMM), 72085 Le Mans Cedex 9, France; and Ecole Nationale Supérieure d’Ingénieurs du Mans (ENSIM), Université du Maine, 72085 Le Mans Cedex 9, France
Marie-Pierre Crosnier-Lopez
Affiliation:
LUNAM Université du Maine, Institut des Molécules et Matériaux du Mans (IMMM), 72085 Le Mans Cedex 9, France
Françoise Le Berre*
Affiliation:
LUNAM Université du Maine, Institut des Molécules et Matériaux du Mans (IMMM), 72085 Le Mans Cedex 9, France
*
a)Address all correspondence to this author. e-mail: francoise.le-berre@univ-lemans.fr
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Abstract

A new acentric protonated garnet Li6−xHxCaLa2Nb2O12 has been synthesized and structurally characterized from Rietveld refinement of high-resolution neutron diffraction data. This phase can be prepared by Li+/H+ exchange on the mother garnet Li6CaLa2Nb2O12 in acetic acid heated at reflux for 4 days, conditions determined after several tests varying acid solution, time, and temperature. Li6−xHxCaLa2Nb2O12 crystallizes in the noncentrosymmetric cubic space group I$\overline 4$3d (no. 220) with the cell parameter a = 12.8040(3) Å. The noncentrosymmetry has been confirmed from unambiguous results obtained by second harmonic generation test as well as from transmission electron microscopy study (selected area electron diffraction). The Li+/H+ exchange corresponds to a topotactic reaction since this new protonated phase is built from the garnet framework [CaLa2Nb2O12]6− like its mother form Li6CaLa2Nb2O12 with lithium and proton cations distributed on different sites.

Type
Articles
Information
Journal of Materials Research , Volume 28 , Issue 16 , 28 August 2013 , pp. 2147 - 2153
Copyright
Copyright © Materials Research Society 2013 

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