Abstract
The crystal structures of two near stoichiometric NASICONS were determined from powder neutron diffraction data. The compound prepared by Hong's solid state reaction had a composition Na 3.17Zr 1.93Si 1.9P 1.1O 12 and a sol-gel preparation heated at 1080°C gave Na 3Zr 1.93Si 2PO 11.86. These compositions, obtained from refinement of the occupancy factors, were found to agree with elemental analysis carried out by X-ray fluorescence. The foregoing compositions are considerably different from that of a NASICON obtained by a hydrothermal route, Na 3.2Zr 1.68Si 1.84P 1.16O 11.54, and their unit cell parameters are somewhat larger. This difference results from the incorporation of approximately 0.32 moles of Na + in the Zr 4+ sites for the hydrothermal preparation. Solid state MAS NMR data are presented to support this finding, and in one sample, trapped electrons were detected. The hypothesis is proposed that the exact stoichiometry of NASICON cannot be represented by a simple solid solution series, but rather, depends on the method of preparation.
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