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DOI: 10.1039/A707130B (Paper) Reference Section for: J. Mater. Chem., 1998, 8, 969-975

Hydrothermal synthesis and crystal structure ofα-LiZnAsO4

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Torben R. Jensen, Poul Norby, Jonathan C. Hanson, Ole Simonsen, Eivind M. Skou, P. C. Stein and Hans A. Bøye

Abstract

Single crystals of lithium zinc arsenate,α-LiZnAsO4 , suitable for structure determination were prepared from an aqueous solution of H3AsO4 , Zn(NO3)2 and LiOH under hydrothermal conditions, at 240 °C. α-LiZnAsO4 has a fully ordered phenacite structure built from a three-dimensional framework of cornersharing AsO4 , ZnO4 and LiO4 tetrahedra. The tetrahedra form nets of six-rings surrounded by six four-rings in the direction of the c-axis. α-LiZnAsO4 crystallises in the trigonal space group R3 (no. 146), a=14.009(2), c=9.386(2) Å, Z=18 and Dc=3.958 g cm–3 . The structure was refined to: wR(F2)=0.130, R(F)=0.050 andS=0.982, for F2>2sigma;(F2). Synchrotron radiation, λ=0.9540 Å, was used for single crystal diffraction giving 917 unique reflections. Solid state 7Li MAS NMR showed a broadened Li signal implying more than one inequivalent Li (δ 0.21, reference: 1.00 mol dm–3 LiCl). Linear thermal expansion coefficients in the temperature range 25–800 °C were determined using time resolved in situ synchrotron X-ray powder diffraction. A weak reversible, possibly second order, thermal event was observed at 682(1) °C using differential scanning calorimetry.

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