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Thermal study on the synthesis of the doped ZnO to be used in TCO films

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Abstract

ZnO, Li doped, and Li, Ni co-doped ZnO powders to be later used as transparent conductive oxide thin film were prepared by heat treatment of gels obtained from alcoholic Zn(CH3COO)2·2H2O, LiNO3·nH2O and NiSO4·6H2O solutions with (CH3CH2OH)3N as chelating agent. The properties of the powders and their thermal treatment were studied by thermogravimetric and differential thermal analysis (TG/DTA), differential scanning calorimetry, evolved gas analysis coupled with mass spectroscopy, Fourier transform infrared spectroscopy, X-ray diffraction and scanning electron microscopy coupled with energy-dispersive X-ray. The as-prepared gels consisted of submicron platelet-like particles and contained zinc acetate dihydrate and hydrozincite in different amount and with different preferred orientations. During annealing of the gels, zinc acetate decomposed between 110 and 350 °C with the release of CH3COOH, acetone and CO2. The N content of the chelating agent was responsible for NH3 and NO evolution. The thermal behavior of the doped gels was similar, but there were also differences in the mass losses, amount of released gases. Based on TG/DTA data, ZnO powders were obtained from the gels by annealing both at 275 and 500 °C. After heating at 275 °C, the obtained powders consisted of spherical 1–2 micron grains of wurtzite. The inclusion of the dopants was successful according to EDX and cell parameter data. Thermal study of the powder annealed at 275 °C confirmed that they still contain some zinc acetate. In the case of the doped samples, the mass loss was smaller, since the Li and Ni dopants catalyzed the composition of zinc acetate during the previous annealing at 275 °C. After annealing the gels at 500 °C, stable undoped ZnO or doped ZnO particles were obtained.

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Acknowledgements

The financial support of EU (ERDF) INFRANANOCHEM-No. 19/01.03.2009 Project is gratefully acknowledged. I.M.S. thanks for a János Bolyai Research Fellowship of the Hungarian Academy of Sciences and an OTKA-PD-109129 Grant. S.B. acknowledges the Postdoctoral Fellowship programme of the Hungarian Academy of Sciences (2013–2015).

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Authors and Affiliations

  1. Institute of Physical Chemistry “Ilie Murgulescu” of the Romanian Academy, 202 Splaiul Independentei, 060021, Bucharest, Romania

    Suzana Mihaiu, Irina Atkinson, Oana Catalina Mocioiu, Jeanina Pandele-Cusu, Alexandra Toader, Cornel Munteanu & Maria Zaharescu

  2. MTA-BME Technical Analytical Chemistry Research Group, Budapest, Szt. Gellért tér 4, 1111, Hungary

    Imre Miklós Szilágyi & Stefan Boyadjiev

  3. Department of Inorganic and Analytical Chemistry, Budapest University of Technology and Economics, Budapest, Szt. Gellért tér 4, 1521, Hungary

    Imre Miklós Szilágyi, Dávid Hunyadi, János Madarász & György Pokol

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  1. Suzana Mihaiu
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  2. Imre Miklós Szilágyi
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  3. Irina Atkinson
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  4. Oana Catalina Mocioiu
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Correspondence to Imre Miklós Szilágyi or Irina Atkinson.

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Mihaiu, S., Szilágyi, I.M., Atkinson, I. et al. Thermal study on the synthesis of the doped ZnO to be used in TCO films. J Therm Anal Calorim 124, 71–80 (2016). https://doi.org/10.1007/s10973-015-5147-2

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  • DOI: https://doi.org/10.1007/s10973-015-5147-2

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