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Synthesis, Crystal Structure, and Stability of Cubic Li 7-x La 3 Zr 2-x Bi x O 12 .
Inorganic Chemistry 2016 December 6
Li oxide garnets are among the most promising candidates for solid-state electrolytes in novel Li ion and Li metal based battery concepts. Cubic Li7 La3 Zr2 O12 stabilized by a partial substitution of Zr4+ by Bi5+ has not been the focus of research yet, despite the fact that Bi5+ would be a cost-effective alternative to other stabilizing cations such as Nb5+ and Ta5+ . In this study, Li7-x La3 Zr2-x Bix O12 (x = 0.10, 0.20, ..., 1.00) was prepared by a low-temperature solid-state synthesis route. The samples have been characterized by a rich portfolio of techniques, including scanning electron microscopy, X-ray powder diffraction, neutron powder diffraction, Raman spectroscopy, and7 Li NMR spectroscopy. Pure-phase cubic garnet samples were obtained for x ≥ 0.20. The introduction of Bi5+ leads to an increase in the unit-cell parameters. Samples are sensitive to air, which causes the formation of LiOH and Li2 CO3 and the protonation of the garnet phase, leading to a further increase in the unit-cell parameters. The incorporation of Bi5+ on the octahedral 16a site was confirmed by Raman spectroscopy.7 Li NMR spectroscopy shows that fast Li ion dynamics are only observed for samples with high Bi5+ contents.
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