A time of flight neutron powder rietveld refinement study at elevated temperature on a monoclinic near-stoichiometric NASICON

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Abstract

Time of flight neutron powder data were collected at elevated temperatures on a sample of NASICON of composition Na3.17Zr1.93Si1.9P1.1O12. This sample, prepared by reheating a commerically available NASICON to minimize the ZrO2impurity, has been previously structurally refined from room temperature neutron diffraction data collected at Argonne National Laboratory. Conductivity measurements show a cusp at ca. 170°C attributed to the monoclinic-rhombohedral transition and the purpose of this work was to explore the nature of the transition. Data runs were made at 143, 173, 202, 300, and 391°C. No evidence for a crystal system change was found. The highest temperature data sets could not be refined satisfactorily by the Rietveld method using a rhombohedral model, but rather required a monoclinic cell in space group C2 c to achieve convergence. An explanation for the conductivity cusp is given in terms of a disordering of the sodium ions and a change in conduction pathways which lowers the barriers to ion movement. © 1988.

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Rudolf, P. R., Clearfield, A., & Jorgensen, J. D. (1988). A time of flight neutron powder rietveld refinement study at elevated temperature on a monoclinic near-stoichiometric NASICON. Journal of Solid State Chemistry, 72(1), 100–112. https://doi.org/10.1016/0022-4596(88)90013-8

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