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Thermal and structural studies of sol–gel-derived yttria-doped ZrO2 nanoparticles

Effect of annealing condition

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Abstract

This investigation focuses on the role of different atmosphere conditions (air and vacuum) during annealing at different temperatures of sol–gel-derived zirconia ZrO2 (stabilised by yttria in 5 mol%) nanocrystals (5YSZ). Prepared samples were characterised by powder X-ray diffraction (PXRD), simultaneous differential thermal and thermogravimetric analysis, evolved gas analysis coupled with mass spectrometry (EGA-MS), Fourier transform infrared spectroscopy (FT-IR) and micro-Raman spectroscopy. The results of thermal analysis and PXRD analysis show the zirconia crystallisation onset at temperature not lower than 400 °C, while EGA-MS analysis further identified gaseous thermal decomposition products. Average crystallite size of the 5YSZ annealed in air at 400, 600, 700 and 800 °C was calculated to be 10, 15, 22 and 33 nm, respectively. On the other hand, crystallite size remains significantly lower when the heat treatment was conducted in vacuum, i.e. in the range 4–13 nm. Annealing atmosphere affects crystallisation, resulting in lower thermal treatment requirements and enabling controlled crystallite growth. PXRD, FT-IR and micro-Raman spectroscopy showed nanocrystalline 5YSZ samples were successfully stabilised in the tetragonal phase and preserved phase stability over the investigated wide thermal treatment range. Due to the yield of stable particle with small size at lower temperatures, the vacuum-prepared 5YSZ coatings are considered as highly applicable for steel corrosion protection.

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Acknowledgements

The financial support of the University of Zagreb is gratefully acknowledged.

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Authors and Affiliations

  1. Forensic Science Centre „Ivan Vučetić“, Ministry of the Interior, Ilica 335, 10 000, Zagreb, Croatia

    Ivana Bačić

  2. Ruđer Bošković Institute, Bijenička cesta 54, 10 000, Zagreb, Croatia

    Vilko Mandić

  3. Faculty of Mechanical Engineering and Naval Architecture, University of Zagreb, Ivana Lučića 5, 10 000, Zagreb, Croatia

    Lidija Ćurković

  4. Faculty of Chemical Engineering and Technology, University of Zagreb, Marulićev trg 19, 10 000, Zagreb, Croatia

    Helena Otmačić-Ćurković & Stanislav Kurajica

Authors
  1. Ivana Bačić
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  2. Vilko Mandić
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  4. Helena Otmačić-Ćurković
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  5. Stanislav Kurajica
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Correspondence to Vilko Mandić.

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Bačić, I., Mandić, V., Ćurković, L. et al. Thermal and structural studies of sol–gel-derived yttria-doped ZrO2 nanoparticles. J Therm Anal Calorim 127, 197–206 (2017). https://doi.org/10.1007/s10973-016-5904-x

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  • DOI: https://doi.org/10.1007/s10973-016-5904-x

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