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Nanoscale Structural Features of Ultra-fine Zirconia Powders Obtained Via Precipitation-hydrothermal Treatment Route

Published online by Cambridge University Press:  15 February 2011

Vladislav A. Sadykov
Affiliation:
Boreskov Institute of Catalysis SB RAS, pr. Lavrentieva, 5, 630090, Novosibirsk, Russia; Novosibirsk State University, Novosibirsk, Russia;
Vladimir I. Zaikovskii
Affiliation:
Boreskov Institute of Catalysis SB RAS, pr. Lavrentieva, 5, 630090, Novosibirsk, Russia;
Dmitrii A. Zyuzin
Affiliation:
Boreskov Institute of Catalysis SB RAS, pr. Lavrentieva, 5, 630090, Novosibirsk, Russia;
Ella M. Moroz
Affiliation:
Boreskov Institute of Catalysis SB RAS, pr. Lavrentieva, 5, 630090, Novosibirsk, Russia;
Elena B. Burgina
Affiliation:
Boreskov Institute of Catalysis SB RAS, pr. Lavrentieva, 5, 630090, Novosibirsk, Russia;
Arcady V. Ishchenko
Affiliation:
Novosibirsk State University, Novosibirsk, Russia;
Vitaly G. Kostrovskii
Affiliation:
Institute of Solid State Chemistry SB RAS, Novosibirsk, Russia.
Valerii A. Matyshak
Affiliation:
Semenov Institute of Chemical Physics RAS, Moscow, Russia.
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Abstract

Genesis of the structure of zirconia fine particles prepared by precipitation of amorphous hydrated zirconia by ammonia from the ZrO(NO3)2 solution followed by a mild hydrothermal treatment (HTT) of precipitate, washing and calcination under air up to 1000 °C has been studied by HRTEM, X-ray diffraction, Raman and FTIRS. HTT rearranges the structure of amorphous zirconia, which helps to obtain nearly single-phase monoclinic nanozirconia (particle size 5-15 nm) after a mild calcination at 500 °C. Dehydroxilation and sintering of these nanoparticles at higher (600-650 °C) temperatures generate polysynthetic (001) twins. Modeling revealed that reappearance of the (111) “cubic” reflex in XRD patterns of samples calcined at 600-650 °C can be due to these extended defects. In their vicinity, the seven-fold Zr-O coordination sphere is retained, while packing of ZrO7 polyhedra is varied towards more symmetric structures, thus causing disappearance of the Raman spectra.

Type
Research Article
Copyright
Copyright © Materials Research Society 2005

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Nanoscale Structural Features of Ultra-fine Zirconia Powders Obtained Via Precipitation-hydrothermal Treatment Route
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