TY - JOUR

T1 - Synthesis of La2Zr2O7 by thermal treatment of mechanically activated salt mixture.

AU - Kalinkin, A. M.

AU - Usol’tsev, A. V.

AU - Kalinkina, E. V.

AU - Chislov, M. V.

AU - Zvereva, I. A.

AU - Nevedomskii, V.N.

N1 - Funding Information: Acknowledgements The thermal analysis was performed at the Centre for Thermogravimetric and Calorimetric Research of the Research Park of St. Petersburg State University. TEM characterization was performed using equipment owned by the Federal Joint Research Center ‘‘Material science and characterization in advanced technology’’ with financial support by Ministry of Education and Science of the Russian Federation (id RFMEFI62117X0018). Financial support within Program No. 5 of the Department of Chemistry and Material Sciences of the Russian Academy of Sciences is gratefully acknowledged. The authors also wish to thank V.V. Semushin for his help in SEM measurements.

PY - 2018/10

Y1 - 2018/10

N2 - A lanthanum zirconate La2Zr2O7 was synthesized by soft mechanochemical method using zirconium oxynitrate ZrO(NO3)2·6H2O and lanthanum carbonate La2(CO3)3·8H2O 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 La2Zr2O7 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.

AB - A lanthanum zirconate La2Zr2O7 was synthesized by soft mechanochemical method using zirconium oxynitrate ZrO(NO3)2·6H2O and lanthanum carbonate La2(CO3)3·8H2O 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 La2Zr2O7 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.

KW - lanthanum zirconate

KW - FTIR spectroscopy

KW - TGA/DSC

KW - Soft mechanochemical synthesis

KW - Exchange reaction

KW - La Zr O

KW - Salt mixture

KW - La2Zr2O7

KW - PRECURSOR

KW - CO2

KW - GEL

KW - POWDERS

KW - PYROCHLORE

KW - LANTHANUM ZIRCONATE

UR - http://www.scopus.com/inward/record.url?scp=85047970671&partnerID=8YFLogxK

UR - http://www.mendeley.com/research/synthesis-la2zr2o7by-thermal-treatment-mechanically-activated-salt-mixture

U2 - 10.1007/s10973-018-7419-0

DO - 10.1007/s10973-018-7419-0

M3 - Article

VL - 134

SP - 111

EP - 118

JO - Journal of Thermal Analysis and Calorimetry

JF - Journal of Thermal Analysis and Calorimetry

SN - 1388-6150

IS - 1

ER -