Synthesis of La2Zr2O7 by thermal treatment of mechanically activated salt mixture

A lanthanum zirconate La 2 Zr 2 O 7 was synthesized by soft mechanochemical method using zirconium oxynitrate ZrO(NO 3 ) 2 ·6H 2 O and lanthanum carbonate La 2 (CO 3 ) 3 ·8H 2 O as reagents. Mechanical activation of the reagents was carried out in a centrifugal planetary ball mill. The processes occ...

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Bibliographic Details
Published in:Journal of thermal analysis and calorimetry 2018-10, Vol.134 (1), p.111-118
Main Authors: Kalinkin, Alexander M., Usol’tsev, Alexander V., Kalinkina, Elena V., Chislov, Mikhail V., Zvereva, Irina A., Nevedomskii, Vladimir N.
Format: Article
Language:English
Subjects:
Activation
Aluminum
Amorphization
Analytical Chemistry
Ball milling
Basic oxides
Chemistry
Chemistry and Materials Science
Crystallization
Exothermic reactions
Fourier transforms
Heat treatment
Inorganic Chemistry
Lanthanum
Mass spectrometry
Measurement Science and Instrumentation
Nitrates
Physical Chemistry
Polymer Sciences
Reagents
Scanning electron microscopy
Synthesis
Transmission electron microscopy
X-ray diffraction
Zirconium oxides
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Summary:A lanthanum zirconate La 2 Zr 2 O 7 was synthesized by soft mechanochemical method using zirconium oxynitrate ZrO(NO 3 ) 2 ·6H 2 O and lanthanum carbonate La 2 (CO 3 ) 3 ·8H 2 O as reagents. Mechanical activation of the reagents was carried out in a centrifugal planetary ball mill. The processes occurring during calcination of the jointly and the separately mechanically activated salt mixture were studied using DSC, TG coupled with mass spectrometry, XRD analysis, and FTIR spectroscopy. It was shown that in the course of joint mechanical activation in the mill alongside with intimate mixing of the reagents and their amorphization exchange reaction occurred, producing lanthanum nitrate, basic lanthanum nitrate, basic zirconium carbonate, and hydrated zirconium oxide. The DSC curve of the jointly mechanically activated salt mixture showed a strong exothermic peak at 878 °C which was not associated with mass loss. This peak was attributed to La 2 Zr 2 O 7 crystallization in agreement with XRD data. Nanocrystalline lanthanum zirconate synthesized by annealing of the jointly mechanically activated salt mixture was characterized using XRD analysis, scanning, and transmission electron microscopy.
ISSN:1388-6150
1588-2926
DOI:10.1007/s10973-018-7419-0