Mixed-Valence Ammonium Trivanadate with a Tunnel Structure Prepared by Pyrolysis of Polyoxovanadate

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  • Haruo Naruke
    Research Laboratory of Resources Utilization, Tokyo Institute of Technology4259 Nagatsuta, Midori-ku, Yokohama 226-8503
  • Toshihiro Yamase
    Research Laboratory of Resources Utilization, Tokyo Institute of Technology4259 Nagatsuta, Midori-ku, Yokohama 226-8503

抄録

<jats:title>Abstract</jats:title> <jats:p>The pyrolysis of a polyoxovanadate solid, (NH4)12[V18O42(H2O)]·nH2O (n ≈ 11), at 300 °C in an Ar+NH3 atmosphere gave a mixed-valence vanadium oxide, (NH4)xV3O7 (x ≈ 0.6), isostructural with Cs0.37V3O7. The crystal structure of (NH4)xV3O7 was refined by the Rietveld method (hexagonal, P63/m, a = 9.8436(6), c = 3.6165(1) Å, V = 303.47(3) Å3, Z = 2). (NH4)xV3O7 comprises edge- and corner-sharing VIV/VO5 square-pyramids with an approximate ratio of VIV : VV ≈ 0.49 : 0.51, to form a columnar cavity along the c-axis, in which ammonium N atoms are hydrogen-bonded to apical O atoms of the VIV/VO5 square-pyramids. A reflux of the (NH4)xV3O7 powder in a 0.6 M LiOH/2-methoxyethanol solution brought about Li-insertion into the columnar cavity without any structural change in the {V3O7} framework.</jats:p>

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