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Title: Time of flight neutron Rietveld refinement study at elevated temperature on a monoclinic near-stoichiometric NASICON

Abstract

Time of flight neutron powder data were collected at elevated temperatures on a sample of NASICON of composition Na/sub 3.17/Zr/sub 1.93/Si/sub 1.9/O/sub 12/. This sample, prepared by reheating a commercially available NASICON to minimize the ZrO/sub 2/ impurity, has been previously structurally refined from room temperature neutron diffraction data collected at Argonne National Laboratory. Conductivity measurements show a cusp at ca. 170/sup 0/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/sup 0/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 disordering of the sodium ions and a change in conduction pathways which lowers the barriers to ion movement.

Authors:
; ;
Publication Date:
Research Org.:
Texas A and M Univ., College Station (USA)
OSTI Identifier:
7078694
DOE Contract Number:  
W-31-109-ENG-38
Resource Type:
Journal Article
Journal Name:
J. Solid State Chem.; (United States)
Additional Journal Information:
Journal Volume: 72:1
Country of Publication:
United States
Language:
English
Subject:
36 MATERIALS SCIENCE; PHOSPHORUS OXIDES; CRYSTAL STRUCTURE; SILICON OXIDES; SODIUM OXIDES; ZIRCONIUM OXIDES; EXPERIMENTAL DATA; NEUTRON DIFFRACTION; POWDERS; SPACE GROUPS; TIME-OF-FLIGHT METHOD; ALKALI METAL COMPOUNDS; CHALCOGENIDES; COHERENT SCATTERING; DATA; DIFFRACTION; INFORMATION; NUMERICAL DATA; OXIDES; OXYGEN COMPOUNDS; PHOSPHORUS COMPOUNDS; SCATTERING; SILICON COMPOUNDS; SODIUM COMPOUNDS; TRANSITION ELEMENT COMPOUNDS; ZIRCONIUM COMPOUNDS; 360202* - Ceramics, Cermets, & Refractories- Structure & Phase Studies

Citation Formats

Rudolf, P R, Clearfield, A, and Jorgensen, J D. Time of flight neutron Rietveld refinement study at elevated temperature on a monoclinic near-stoichiometric NASICON. United States: N. p., 1988. Web. doi:10.1016/0022-4596(88)90013-8.
Rudolf, P R, Clearfield, A, & Jorgensen, J D. Time of flight neutron Rietveld refinement study at elevated temperature on a monoclinic near-stoichiometric NASICON. United States. https://doi.org/10.1016/0022-4596(88)90013-8
Rudolf, P R, Clearfield, A, and Jorgensen, J D. Fri . "Time of flight neutron Rietveld refinement study at elevated temperature on a monoclinic near-stoichiometric NASICON". United States. https://doi.org/10.1016/0022-4596(88)90013-8.
@article{osti_7078694,
title = {Time of flight neutron Rietveld refinement study at elevated temperature on a monoclinic near-stoichiometric NASICON},
author = {Rudolf, P R and Clearfield, A and Jorgensen, J D},
abstractNote = {Time of flight neutron powder data were collected at elevated temperatures on a sample of NASICON of composition Na/sub 3.17/Zr/sub 1.93/Si/sub 1.9/O/sub 12/. This sample, prepared by reheating a commercially available NASICON to minimize the ZrO/sub 2/ impurity, has been previously structurally refined from room temperature neutron diffraction data collected at Argonne National Laboratory. Conductivity measurements show a cusp at ca. 170/sup 0/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/sup 0/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 disordering of the sodium ions and a change in conduction pathways which lowers the barriers to ion movement.},
doi = {10.1016/0022-4596(88)90013-8},
url = {https://www.osti.gov/biblio/7078694}, journal = {J. Solid State Chem.; (United States)},
number = ,
volume = 72:1,
place = {United States},
year = {1988},
month = {1}
}