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Thermogravimetric study on preparation of NiTiO3 in different reaction times

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Abstract

The thermodynamic properties of the fabrication of NiTiO3 material in different reaction times are reported. The design of this material is accessible through a new efficient sol–gel methods, utilizing Ni(Ac)2·4H2O and Ti(OiPr)4 as starting materials for the formation of NiTiO3 final product through thermal decomposition. The thermogravimetric (TG) and differential scanning calorimetric (DSC) techniques were used to analyze the reaction of Ni(Ac)2·4H2O and Ti(OiPr)4, which produces precursor materials at 0.5, 1, 2, 24, 48 and 72 h of reaction times, as well as the thermal stability of these precursors and the final product. The DSC data show an exothermic phenomenon of releasing large amount of energy of −1393 J/g at T Peak 655 K due to the first event of decomposition started at T Onset 607 K and finished at T Endset 663 K for the precursor materials obtained at 0.5 h of reaction, showing the presence of starting materials in this precursor. A similar exothermic behavior was observed in the sample of 1 h of reaction time and was vanished in the materials obtained at 2–72 h of reaction, indicating the influence of the time on the completion of reaction and formation of NiTiO3 crystalline phase as final product of thermal decomposition. In addition, using the information obtained from the TG/DSC, XRD and FTIR analyses, the optimum temperature for the thermal decomposition of the precursor materials to NiTiO3 with fairly high crystallinity was also determined and discussed.

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Acknowledgements

Laboratory of Thermal Analysis Prof. Ivo Giolito (Latig–USP) and the Laboratory of the f Block Elements (LEB-f) to measures of TG/DSC, Núcleo de Petróleo (Labpetro—UFES) to measures of FTIR and funding agency Coordenação de Apoio a Amparo a Pesquisa (CAPES).

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Authors and Affiliations

  1. Department of Fundamental Chemistry, Institute of Chemistry, University of São Paulo, São Paulo, SP, Brazil

    R. V. Rodrigues, L. U. Khan, J. R. Matos & H. F. Brito

  2. Department of Chemistry, Federal University of Espírito Santo, Vitória, ES, Brazil

    R. V. Rodrigues, E. J. B. Muri, A. A. L. Marins, R. M. Oliveira & L. C. Machado

  3. Department of Physics, Federal University of Espírito Santo, Vitória, ES, Brazil

    P. C. M. da Cruz

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  1. R. V. Rodrigues
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  2. E. J. B. Muri
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  3. P. C. M. da Cruz
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  4. A. A. L. Marins
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Rodrigues, R.V., Muri, E.J.B., da Cruz, P.C.M. et al. Thermogravimetric study on preparation of NiTiO3 in different reaction times. J Therm Anal Calorim 126, 1499–1505 (2016). https://doi.org/10.1007/s10973-016-5836-5

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  • DOI: https://doi.org/10.1007/s10973-016-5836-5

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