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Title: The crystal structure of a nonstoichiometric nasicon

Abstract

The crystal structure of a nonstoichiometric NASICON prepared from a hydrothermally synthesized precursor phase was solved by means of Xray powder and neutron powder diffraction methods. The NASICON phase is monoclinic with unit cell parameters, from Rietveld refinement of the neutron data, of a = 15.6209(8), b = 9.0326(5), c = 9.2172(5)A, ..beta.. = 123.67(1)A, V = 1082.5A/sup 3/. The space group is C2/c with Z = 4. The structure is essentially that proposed earlier by Hong, but the nonstoichiometry results from replacement of part of the Zr/sup 4 +/ by Na/sup +/. Refinement of site occupancies coupled with the requirement of overall charge balance yields the formula Na /sub 2.88/ (Na /sub 0.32/ Zr /sub 1.68/ )Si /sub 1.84/ P /sub 1.16/ O /sub 11.54/ which also agrees well with analytical data. Only 20% of the Na1 sites are occupied, but 80% of the Na3 sites are filled. This structure provides a framework from which to rationalize the many reports in the literature that NASICON can only be prepared with difficulty by high temperature solid state reactions.

Authors:
; ; ;
Publication Date:
Research Org.:
Department of Chemistry, Texas A and M University, College Station, Texas
OSTI Identifier:
6407209
Resource Type:
Journal Article
Journal Name:
Mater. Res. Bull.; (United States)
Additional Journal Information:
Journal Volume: 20:6
Country of Publication:
United States
Language:
English
Subject:
36 MATERIALS SCIENCE; SILICON COMPOUNDS; CHEMICAL PREPARATION; CRYSTALLOGRAPHY; SODIUM COMPOUNDS; CHEMICAL COMPOSITION; CRYSTAL STRUCTURE; CRYSTAL-PHASE TRANSFORMATIONS; DIFFRACTION; HEAT TREATMENTS; OXYGEN COMPOUNDS; PHASE STUDIES; PHOSPHORUS COMPOUNDS; SOLID STATE PHYSICS; ZIRCONIUM COMPOUNDS; ALKALI METAL COMPOUNDS; COHERENT SCATTERING; PHASE TRANSFORMATIONS; PHYSICS; SCATTERING; SYNTHESIS; TRANSITION ELEMENT COMPOUNDS; 360601* - Other Materials- Preparation & Manufacture; 360602 - Other Materials- Structure & Phase Studies

Citation Formats

Rudolf, F, Clearfield, A, Jorgensen, J D, and Subramanian, M A. The crystal structure of a nonstoichiometric nasicon. United States: N. p., 1985. Web. doi:10.1016/0025-5408(85)90142-4.
Rudolf, F, Clearfield, A, Jorgensen, J D, & Subramanian, M A. The crystal structure of a nonstoichiometric nasicon. United States. https://doi.org/10.1016/0025-5408(85)90142-4
Rudolf, F, Clearfield, A, Jorgensen, J D, and Subramanian, M A. 1985. "The crystal structure of a nonstoichiometric nasicon". United States. https://doi.org/10.1016/0025-5408(85)90142-4.
@article{osti_6407209,
title = {The crystal structure of a nonstoichiometric nasicon},
author = {Rudolf, F and Clearfield, A and Jorgensen, J D and Subramanian, M A},
abstractNote = {The crystal structure of a nonstoichiometric NASICON prepared from a hydrothermally synthesized precursor phase was solved by means of Xray powder and neutron powder diffraction methods. The NASICON phase is monoclinic with unit cell parameters, from Rietveld refinement of the neutron data, of a = 15.6209(8), b = 9.0326(5), c = 9.2172(5)A, ..beta.. = 123.67(1)A, V = 1082.5A/sup 3/. The space group is C2/c with Z = 4. The structure is essentially that proposed earlier by Hong, but the nonstoichiometry results from replacement of part of the Zr/sup 4 +/ by Na/sup +/. Refinement of site occupancies coupled with the requirement of overall charge balance yields the formula Na /sub 2.88/ (Na /sub 0.32/ Zr /sub 1.68/ )Si /sub 1.84/ P /sub 1.16/ O /sub 11.54/ which also agrees well with analytical data. Only 20% of the Na1 sites are occupied, but 80% of the Na3 sites are filled. This structure provides a framework from which to rationalize the many reports in the literature that NASICON can only be prepared with difficulty by high temperature solid state reactions.},
doi = {10.1016/0025-5408(85)90142-4},
url = {https://www.osti.gov/biblio/6407209}, journal = {Mater. Res. Bull.; (United States)},
number = ,
volume = 20:6,
place = {United States},
year = {1985},
month = {6}
}