Depending on the sintering conditions the reactivity of Li₂SnO₃ is different. For Li₂SnO₃ annealed at 700°C the extent of the exchange of Li⁺ ions for hydrogen, realized through the formation of Li_2-xH_xSnO₃, is about x=1.8, whereas for precursors annealed at 900-1100°C x ≤ 0.3. In order to clear up the origin of this fact, a structural investigation of low-temperature Li₂SnO₃ has been carried out.

A stoichiometric mixture of SnO₂ and Li₂CO₃ (99.9 %) were annealed at temperatures up to 700ºC during 48 h. X-ray and neutron powder data yielded for Li₂SnO₃ the monoclinic unit cell, sp. gr. C2/c, parameters: a = 5.3033(2)Å, b = 9.1738(3)Å, c = 10.0195(2)Å, β = 100.042(2)°. In the electron diffraction patterns of Li₂SnO₃ taken along the [100]* direction lines of diffuse scattering have been observed. Random stacking of LiSn₂O₆ slabs shifted either over [1/2 0 0] or [1/2 1/6 0] or [0 1/6 0] can cause the appearance of diffuse intensity along c*. In order to check this assumption, simulations of X-ray and neutron powder diffraction data were performed with the DISCUS software package [1]. The best fit with the experimental patterns has been found for the model with a stacking displacement of ab planes over [1/2 1/6 0] with a propability of 45%. This displacement, which is equivalent to 120° rotational stacking faults was confirmed by the presence of extra spots on the ED patterns and higher intensities for (0h0), (hhl) and (-hhl) reflection series in the X-ray powder diffraction patterns. Diffraction experiments and DISCUS simulations of defect models reveal two kinds of disorder in this material: domains in ab planes and stacking disorder along the c-axis.

[1] Proffen Th., Neder R.B., J. Appl. Crystallogr. 30 (1997) 171-175

This work was supported by the RFBR (grant no. 06-08-00847), by Belgium Science Policy, by the Council for Grants of the President of the Russian Federation for Support of Leading Scientific Schools (grant no. NSh - 1170.2008.3).

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