The preparation of NASICON powders has been achieved by sol-gel methods. The precursor solution was either rapidly hydrolyzed, to get a precipitate, or slowly gelated under exposure to atmospheric humidity. The slow hydrolysis process was studied using nuclear magnetic resonance (NMR) spectroscopy in liquid phase. Two-dimensional experiments indicate the occurrence of ligand exchange reactions in solution. Monodimensional H-1, C-13, P-31, and Na-23 NMR spectra were also measured. NMR allowed us to follow the advancement of the reaction and determine the degree of polymerization. NASICON powders having the Na3Zr2Si2PO12 composition were prepared by heating both precursors at various temperatures in the range 800-1200 degrees C for 1 h. The phase evolution as a function of the decomposition temperature was investigated by simultaneous thermogravimetric and differential thermal analysis (TG-DTA) and X-ray diffraction (XRD) analysis. The NASICON prepared by fast hydrolysis contained a larger amount of free zirconia, while the samples prepared by slow hydrolysis were almost pure, showing a monoclinic structure.

DI VONA, M.l., Licoccia, S., Montanaro, L., Traversa, E. (1999). Sol-gel synthesis of NASICON: 1D and 2D NMR investigation. CHEMISTRY OF MATERIALS, 11(5), 1336-1341 [10.1021/cm9807788].

Sol-gel synthesis of NASICON: 1D and 2D NMR investigation

DI VONA, MARIA LUISA;LICOCCIA, SILVIA;TRAVERSA, ENRICO
1999-01-01

Abstract

The preparation of NASICON powders has been achieved by sol-gel methods. The precursor solution was either rapidly hydrolyzed, to get a precipitate, or slowly gelated under exposure to atmospheric humidity. The slow hydrolysis process was studied using nuclear magnetic resonance (NMR) spectroscopy in liquid phase. Two-dimensional experiments indicate the occurrence of ligand exchange reactions in solution. Monodimensional H-1, C-13, P-31, and Na-23 NMR spectra were also measured. NMR allowed us to follow the advancement of the reaction and determine the degree of polymerization. NASICON powders having the Na3Zr2Si2PO12 composition were prepared by heating both precursors at various temperatures in the range 800-1200 degrees C for 1 h. The phase evolution as a function of the decomposition temperature was investigated by simultaneous thermogravimetric and differential thermal analysis (TG-DTA) and X-ray diffraction (XRD) analysis. The NASICON prepared by fast hydrolysis contained a larger amount of free zirconia, while the samples prepared by slow hydrolysis were almost pure, showing a monoclinic structure.
Pubblicato
Rilevanza internazionale
Articolo
Sì, ma tipo non specificato
Settore CHIM/07 - Fondamenti Chimici delle Tecnologie
Settore ING-IND/22 - Scienza e Tecnologia dei Materiali
English
Con Impact Factor ISI
CARBON-DIOXIDE SENSOR; P-31 MAS NMR; PHASE-TRANSFORMATION; CERAMICS; CHEMISTRY; ELECTRODE; SYSTEM; NA-23
DI VONA, M.l., Licoccia, S., Montanaro, L., Traversa, E. (1999). Sol-gel synthesis of NASICON: 1D and 2D NMR investigation. CHEMISTRY OF MATERIALS, 11(5), 1336-1341 [10.1021/cm9807788].
DI VONA, Ml; Licoccia, S; Montanaro, L; Traversa, E
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Utilizza questo identificativo per citare o creare un link a questo documento: https://hdl.handle.net/2108/44040
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