Nonhydrolytic synthesis of NASICON of composition Na3Zr2Si2PO12: A spectroscopic study

M. L. Di Vona; E. Traversa; S. Licoccia

doi:10.1021/cm001128i

Nonhydrolytic synthesis of NASICON of composition Na₃Zr₂Si₂PO₁₂: A spectroscopic study

M. L. Di Vona^*, E. Traversa, S. Licoccia

^*Corresponding author for this work

Research output: Contribution to journal › Article › peer-review

19 Scopus citations

Abstract

NASICON (Na₃Zr₂Si₂PO₁₂) has been prepared by a nonhydrolytic route reacting OP(OBu)₃, SiCl₄, Zr(Ot-Bu)₄, and NaOt-Bu in acetonitrile. The progress of the reaction was monitored by measuring ³¹P and ¹³C NMR spectra in the liquid phase and mass spectra of the reaction mixture. The spectroscopic analysis allowed optimization of the synthetic conditions. The thermal decomposition behavior of the precursor was studied by simultaneous thermogravimetric and differential thermal analysis. The NASICON precursor was heated to selected temperatures, and the resulting powders were analyzed by X-ray diffraction to check the formation of the NASICON phase. The powder obtained at 900 °C was almost pure, showing only traces of free zirconia.

Original language	English (US)
Pages (from-to)	141-144
Number of pages	4
Journal	Chemistry of Materials
Volume	13
Issue number	1
DOIs	https://doi.org/10.1021/cm001128i
State	Published - 2001
Externally published	Yes

ASJC Scopus subject areas

General Chemistry
General Chemical Engineering
Materials Chemistry

Access to Document

10.1021/cm001128i

Cite this

@article{ac56659e9d9749598a7311989a55c2dd,

title = "Nonhydrolytic synthesis of NASICON of composition Na3Zr2Si2PO12: A spectroscopic study",

abstract = "NASICON (Na3Zr2Si2PO12) has been prepared by a nonhydrolytic route reacting OP(OBu)3, SiCl4, Zr(Ot-Bu)4, and NaOt-Bu in acetonitrile. The progress of the reaction was monitored by measuring 31P and 13C NMR spectra in the liquid phase and mass spectra of the reaction mixture. The spectroscopic analysis allowed optimization of the synthetic conditions. The thermal decomposition behavior of the precursor was studied by simultaneous thermogravimetric and differential thermal analysis. The NASICON precursor was heated to selected temperatures, and the resulting powders were analyzed by X-ray diffraction to check the formation of the NASICON phase. The powder obtained at 900 °C was almost pure, showing only traces of free zirconia.",

author = "{Di Vona}, {M. L.} and E. Traversa and S. Licoccia",

year = "2001",

doi = "10.1021/cm001128i",

language = "English (US)",

volume = "13",

pages = "141--144",

journal = "Chemistry of Materials",

issn = "0897-4756",

publisher = "AMER CHEMICAL SOC",

number = "1",

}

TY - JOUR

T1 - Nonhydrolytic synthesis of NASICON of composition Na3Zr2Si2PO12

T2 - A spectroscopic study

AU - Di Vona, M. L.

AU - Traversa, E.

AU - Licoccia, S.

PY - 2001

Y1 - 2001

N2 - NASICON (Na3Zr2Si2PO12) has been prepared by a nonhydrolytic route reacting OP(OBu)3, SiCl4, Zr(Ot-Bu)4, and NaOt-Bu in acetonitrile. The progress of the reaction was monitored by measuring 31P and 13C NMR spectra in the liquid phase and mass spectra of the reaction mixture. The spectroscopic analysis allowed optimization of the synthetic conditions. The thermal decomposition behavior of the precursor was studied by simultaneous thermogravimetric and differential thermal analysis. The NASICON precursor was heated to selected temperatures, and the resulting powders were analyzed by X-ray diffraction to check the formation of the NASICON phase. The powder obtained at 900 °C was almost pure, showing only traces of free zirconia.

AB - NASICON (Na3Zr2Si2PO12) has been prepared by a nonhydrolytic route reacting OP(OBu)3, SiCl4, Zr(Ot-Bu)4, and NaOt-Bu in acetonitrile. The progress of the reaction was monitored by measuring 31P and 13C NMR spectra in the liquid phase and mass spectra of the reaction mixture. The spectroscopic analysis allowed optimization of the synthetic conditions. The thermal decomposition behavior of the precursor was studied by simultaneous thermogravimetric and differential thermal analysis. The NASICON precursor was heated to selected temperatures, and the resulting powders were analyzed by X-ray diffraction to check the formation of the NASICON phase. The powder obtained at 900 °C was almost pure, showing only traces of free zirconia.

UR - http://www.scopus.com/inward/record.url?scp=0035111533&partnerID=8YFLogxK

U2 - 10.1021/cm001128i

DO - 10.1021/cm001128i

M3 - Article

AN - SCOPUS:0035111533

SN - 0897-4756

VL - 13

SP - 141

EP - 144

JO - Chemistry of Materials

JF - Chemistry of Materials

IS - 1

ER -

Nonhydrolytic synthesis of NASICON of composition Na₃Zr₂Si₂PO₁₂: A spectroscopic study

Abstract

ASJC Scopus subject areas

Access to Document

Other files and links

Fingerprint

Cite this