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Low-temperature synthesis and thermal expansion of nanocrystalline monoclinic zirconolite ceramics

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Abstract

The nanocrystalline Zirconolite (CaZrTi2O7 or CZT) powder was successfully synthesized at low temperature using wet chemical method. The calcination temperature was estimated by simultaneous thermogravimetry and differential thermal analysis (TG–DTA). The calcination of the precursor at the various temperatures (600–1250 °C) exhibited two major phases of nanocrystalline CZT powder. The XRD pattern has confirmed the formation of the fluorite structure at 600–900 °C. However, the fluorite structure of the CZT was completely transformed to monoclinic (2 M) structure at 1000 °C. Further, SEM, and TEM have investigated the influence of annealing temperatures on the microstructures and particle size. The linear thermal expansion of sintered CZT pellet was measured by dilatometrically in the range of 30–950 °C and the calculated thermal expansion coefficient value was (α) = 9.93 × 10–6 K−1. The theoretical density > 95% was achieved in nanocrystalline CZT powder after being pelletized and sintered at 1250 °C for 5 h. The thermal expansion coefficient and density of the CZT are favorable for potential application in the immobilization of radwaste containing actinide and lanthanides.

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Acknowledgements

The SAIF facilities, IIT-B Mumbai and NCNNUM, University of Mumbai are specially acknowledged for their characterization facilities such as SEM, TEM and TGA etc. Mr. Harishchandra Nishad from NCNNUM has been acknowledged for SAED pattern indexing.

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Authors and Affiliations

  1. Department of Chemistry, Institute of Science, 15-Madam Cama Road, Mumbai, 400032, India

    Bhimarao M. Patil

  2. Karmaveer Bhaurao Patil College, VashiNavi Mumbai, 400703, India

    Gurumeet C. Wadhawa

  3. National Centre for Nanosciences and Nanotechnology, University of Mumbai, Mumbai, 400098, India

    Atul C. Chaskar & Pravin S. Walke

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  1. Bhimarao M. Patil
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BMP performed the synthesis and characterization and wrote the manuscript. GCW, ACC and PSW corrected the manuscript. All authors discussed the results, helped shape the research as well as read and approved the final manuscript.

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Correspondence to Bhimarao M. Patil.

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Patil, B.M., Wadhawa, G.C., Chaskar, A.C. et al. Low-temperature synthesis and thermal expansion of nanocrystalline monoclinic zirconolite ceramics. J Therm Anal Calorim 148, 7591–7596 (2023). https://doi.org/10.1007/s10973-023-12269-z

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