Preparation of NASICON Silico Phosphates of Composition Na1 + xZr2SixP3 – xO12 by Pyrolysis of Solution in Melt

A new method for preparing Na 1 + x Zr 2 Si x P 3 – x O 12 (0 < x < 3) based on pyrolysis of solution containing a mixture of organic components in rosin melt has been proposed. Effect of superstoichiometric amounts of sodium and phosphorus on the phase composition of synthesis products has be...

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Bibliographic Details
Published in:Russian journal of inorganic chemistry 2023-08, Vol.68 (8), p.972-978
Main Authors: Grishchenko, D. N., Medkov, M. A.
Format: Article
Language:English
Subjects:
Admixtures
Chemistry
Chemistry and Materials Science
Inorganic Chemistry
Phase composition
Phosphates
Precursors
Pyrolysis
Rosin
Silicon
Sodium
Synthesis
Synthesis and Properties of Inorganic Compounds
X ray powder diffraction
Zirconium
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Summary:A new method for preparing Na 1 + x Zr 2 Si x P 3 – x O 12 (0 < x < 3) based on pyrolysis of solution containing a mixture of organic components in rosin melt has been proposed. Effect of superstoichiometric amounts of sodium and phosphorus on the phase composition of synthesis products has been proved. It has been found that precursor for the sample of maximal purity of phase composition is prepared at molar ratio Na : Zr : Si : P = (1.15 + x ) : 2 : x : ( y – x ), where y = 3 (1.20 + x )/(1 + x ). Precursor calcination temperature is 1000°C. Different NASICON compositions without crystalline admixtures have been obtained in the range 1.5 ≤ x ≤ 2.12. The prepared samples have been studied by X-ray powder diffraction and scanning electron microscopy. The disclosed method of synthesis is promising for the preparation of NASICON as both bulk materials and thin layer coatings.
ISSN:0036-0236
1531-8613
DOI:10.1134/S003602362360123X