Journal of Materials Science

, Volume 31, Issue 17, pp 4581–4589 | Cite as

Characterization of mono- and diphasic mullite precursor powders prepared by aqueous routes. 27Al and 29Si MAS-NMR spectroscopy investigations

  • I. Jaymes
  • A. Douy
  • D. Massiot
  • J. P. Coutures


The structural evolution from amorphous to crystalline mullite, for different 3Al2O3 · 2SiO2 mono- and diphasic precursors, has been investigated by 29Si and 27Al magic angle spinning nuclear magnetic resonance (MAS NMR) spectroscopy. The crystallization has also been studied by X-ray diffraction (XRD) and differential scanning calorimetry (DSC). The chemical composition in the aluminosilicate network of the diphasic precursors and in the crystallized phases has been determined from the 29Si NMR spectra. A close agreement is found with the composition deduced from the lattice parameters measured by XRD. For monophasic precursors the amount of hexa-coordinated aluminium atoms decreases when the temperature increases while Al(IV) and Al(V) increase. Al(VI) practically completely disappears just before the crystallization at 980 °C. An alumina-rich mullite 2Al2O3 · SiO2 (2∶1 mullite) is then formed through a strong exotherm. An enthalpy of 75 kJ per mol is determined for the crystallization of the 2∶1 mullite. At higher temperatures the segregated silica is progressively reincorporated into the mullite lattice. For diphasic precursors the 29Si NMR spectroscopy shows the segregation of silica. The aluminosilicate network is then richer in alumina and the amount of remaining AlO6 octahedra before the crystallization at 980 °C is higher. Spinel crystallizes and continues to become richer in alumina until it reacts with silica to form the stoichiometric 3∶2 mullite at 1260–1275 °C. The nature of the crystallization is related to the local composition of the amorphous alumino-silicate network and to the amount of AlO6 octahedra on approaching 980 °C.


Crystallization Nuclear Magnetic Resonance Differential Scanning Calorimetry Aluminium Atom Precursor Powder 
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Copyright information

© Chapman & Hall 1996

Authors and Affiliations

  • I. Jaymes
    • 1
  • A. Douy
    • 1
  • D. Massiot
    • 1
  • J. P. Coutures
    • 1
  1. 1.CNRS-Centre de Recherches sur la Physique des Hautes TempératuresOrléans Cedex 02France

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