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 29.10.2010   Карта сайта     Language По-русски По-английски
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29.10.2010





Synthesis, structural characterization and Li+ ion conductivity of a new vanado-molybdate phase, LiMg3VMo2O12





Lisa J. Gilliea, Corresponding Author Contact Information, E-mail The Corresponding Author, Sharon A. de Souzab, Denis Sheptyakovc, Nik Reeves-McLarenb, Denis Paserob and Anthony R. Westb






a Department of Chemical and Biological Sciences, School of Applied Sciences, University of Huddersfield, Queensgate, Huddersfield HD1 3DH, UK


b Department of Engineering Materials, Sir Robert Hadfield Building, University of Sheffield, Mappin Street, Sheffield S1 3JD, UK


c Laboratory for Neutron Scattering, ETHZ&PSI, CH-5232 Villigen PSI, Switzerland





Received 5 July 2010; 


revised 27 August 2010; 


accepted 31 August 2010. 


Available online 8 September 2010.









Abstract



A new vanado-molybdate LiMg3VMo2O12 has been synthesized, the crystal structure determined an ionic conductivity measured. The solid solution Li2−zMg2+zVzMo3−zO12 was investigated and the structures of the z=0.5 and 1.0 compositions were refined by Rietveld analysis of powder X-ray (XRD) and powder neutron diffraction (ND) data. The structures were refined in the orthorhombic space group Pnma with anot, vert, similar5.10, bnot, vert, similar10.4 and cnot, vert, similar17.6 Å, and are isostructural with the previously reported double molybdates Li2M2(MoO4)3 (M=M2+, z=0). The structures comprise of two unique (Li/Mg)O6 octahedra, (Li/Mg)O6 trigonal prisms and two unique (Mo/V)O4 tetrahedra. A well-defined 1:3 ratio of Li+:Mg2+ is observed in octahedral chains for LiMg3VMo2O12. Li+ preferentially occupies trigonal prisms and Mg2+ favours octahedral sheets. Excess V5+ adjacent to the octahedral sheets may indicate short-range order. Ionic conductivity measured by impedance spectroscopy (IS) and differential scanning calorimetry (DSC) measurements show the presence of a phase transition, at 500–600 °C, depending on x. A decrease in activation energy for Li+ ion conductivity occurs at the phase transition and the high temperature structure is a good Li+ ion conductor, with σ=1×10−3–4×10−2 S cm−1 and Ea=0.6 to 0.8 eV.









graphical Abstract



A new vanado-molybdate LiMg3VMo2O12 has been synthesized and the crystal structure determined. Ionic conductivity measurements show the presence of a phase transition, at 500–600 °C. A large decrease in activation energy for Li+ ion conductivity occurs at the phase transition and the high temperature structure is a good Li+ ion conductor.

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