Abstract
The structure of γ-Li 3AsO 4 has been refined by Rietveld analysis of high resolution powder neutron diffraction data collected at 770 and 850°C. The structure is related to that of γ-Li 3PO 4, being a distorted hexagonal close-packed arrangement of oxide ions with half the tetrahedral sites filled by cations. Arsenic occupies the same sites as phosphorus in γ-Li 3PO 4, Li + ions show positional disorder; Li(1) ions are split into central and off-center positions within their tetrahedral sites; Li(2) ions are distributed over pairs of face sharing tetrahedral sites at 850°C while occupying only one site at 770°C. The powder neutron data show anisotropic broadening of hkl peaks with h = 2n + 1. The broadening has been accounted for using a modified Rietveld code. The broadened peaks correspond to those reflections that are not common to the related low temperature β-phase and are associated with a doubling of the a-axis during the β-γ transition. The origin of the broadening is the small size of the γ-phase domains in the a -direction; adjacent domains are probably connected by antiphase boundaries.
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