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29Si nuclear-magnetic-resonance and vibrational spectroscopy studies of SiO2–TiO2 powders prepared by the sol-gel process

Published online by Cambridge University Press:  31 January 2011

J. P. Rainho ,
J. Rocha ,
L. D. Carlos  and
R. M. Almeida
J. P. Rainho
Affiliation:
Departments of Physics and Chemistry, University of Aveiro, 3810–193 Aveiro, Portugal
J. Rocha
Affiliation:
Department of Chemistry, University of Aveiro, 3810–193 Aveiro, Portugal
L. D. Carlos
Affiliation:
Department of Physics, University of Aveiro, 3810–193 Aveiro, Portugal
R. M. Almeida
Affiliation:
Department of Materials Engineering, Institut de Engenharia de Sistemas e Computadores (INESC) Investigaçáo e Desenvolvimento (ID), Instituto Superior Técnico, Av. Rovisco Pais, 1000–049 Lisbon, Portugal
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Abstract

The sol-gel synthesis and structural characterization of SiO2–TiO2 powders are reported. Samples with titania concentrations in the range of 0 to 30 mol%, calcined at temperatures between 120 and 1300 °C, were characterized by 29Si magic-angle-spinning nuclear-magnetic-resonance (MAS NMR) and cross polarization MAS NMR, Raman and Fourier transform infrared spectroscopies, and powder x-ray diffraction. Tetrahedrally coordinated Ti (IV) ions were found in the titanosilicate matrix. When the titania content increases beyond approximately 10 mol% and upon calcination at temperatures over approximately 700 °C, the segregation of an amorphous silica-rich phase occurs, together with the precipitation of anatase nanocrystallites with average sizes between 3 and 17 nm, depending on the temperature. An increase in the heat treatment temperature, or the titania content, leads to an increase in the degree of homocondensation (Si–O–Si and Ti–O–Ti bonds) and a simultaneous reduction in the degree of heterocondensation (Si–O–Ti bonds).

Type
Articles
Information
Journal of Materials Research , Volume 16 , Issue 8 , August 2001 , pp. 2369 - 2376
Copyright
Copyright © Materials Research Society 2001

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