Spectroscopic monitoring of sol-gel syntheses of heterometallic ceramics

Silvia Licoccia*, Enrico Traversa, Maria Luisa Di Vona

*Corresponding author for this work

Research output: Contribution to journalArticlepeer-review

2 Scopus citations

Abstract

Multinuclear NMR spectroscopy and mass spectrometry have been used to monitor the sol-gel syntheses of heterometallic ceramics. Hydrolytic and non-hydrolytic sol-gel procedures have been used for the synthesis of NASICON, Na3Zr2Si2PO12. In the hydrolytic process the precursors were slowly gelated under exposure to atmospheric moisture. 1D and 2D NMR measurement allowed to follow the advancement of the reaction and determine the degree of polymerization. In the non-hydrolytic process the spectroscopic analysis allowed to establish the reaction mechanism and to optimize the synthetic conditions. After thermal treatments a very high quality NASICON phase has been obtained as shown by XRD. Three different procedures have been used with the aim of preparing thin films of β-Al2TiO5 by hydrolysis of alkoxides of the two metals in acidic condition with or without 2,4-pentanedione (acac) as a chelating agent. Both NMR and MS indicated as the best synthesis the one carried out without acac. XRD patterns of the films obtained confirmed the results of the spectroscopic analysis.

Original languageEnglish (US)
Pages (from-to)119-124
Number of pages6
JournalJournal of Sol-Gel Science and Technology
Volume26
Issue number1-3
DOIs
StatePublished - Jan 1 2003

Keywords

  • Aluminum titanate
  • Mass spectrometry
  • NASICON
  • NMR spectroscopy

ASJC Scopus subject areas

  • Ceramics and Composites

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