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The Effect of sulfating on the Crystalline Structure of Sol-Gel Zirconia Nanophases

Published online by Cambridge University Press:  10 February 2011

Bokhimi
Affiliation:
Institute of Physics, UNAM, A. P. 20–364, 01000 México D. F., Mexico, bokhimi@sysul2.ifisicacu.unam.mx.
A. Morales
Affiliation:
Institute of Physics, UNAM, A. P. 20–364, 01000 México D. F., Mexico, bokhimi@sysul2.ifisicacu.unam.mx.
O. Novaro
Affiliation:
Institute of Physics, UNAM, A. P. 20–364, 01000 México D. F., Mexico, bokhimi@sysul2.ifisicacu.unam.mx.
M. Portilla
Affiliation:
Faculty of Chemistry, UNAM, A. P. 70–197, 01000 Mexico D. F., Mexico.
T. Lopez
Affiliation:
Faculty of Chemistry, UAM-I, A. P. 54–534, 09340 Mexico D. F., Mexico.
F. Tzompantzi
Affiliation:
Faculty of Chemistry, UAM-I, A. P. 54–534, 09340 Mexico D. F., Mexico.
R. Gomez
Affiliation:
Faculty of Chemistry, UAM-I, A. P. 54–534, 09340 Mexico D. F., Mexico.
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Abstract

Nanophases of sol-gel zirconia were prepared with HCl, C2H4O2 and NH4OH as hydrolysis catalysts, and sulfated with H2SO4. They were analyzed by using X-ray powder diffraction, and their crystalline structure was refined by using the Rietveld method. All samples annealed below 300 °C were amorphous. The non-sulfated samples crystallized around 350 °C, while the sulfated samples crystallized around 600 °C, when they started loosing sulfate ions. In the initial stage of crystallization, both the tetragonal and monoclinic nanophases coexisted, with the tetragonal as the main phase. Annealing the samples at higher temperatures transformed the tetragonal nanophase, stabilized by OH ions, into the monoclinic one.

Type
Research Article
Copyright
Copyright © Materials Research Society 1997

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