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Journal of Thermal Analysis and Calorimetry

, Volume 107, Issue 2, pp 681–691 | Cite as

An in-depth in situ IR study of the thermal decomposition of yttrium trifluoroacetate hydrate

  • M. Mosiadz
  • K. L. Juda
  • S. C. Hopkins
  • J. Soloducho
  • B. A. Glowacki
Article

Abstract

The pyrolysis of Y(CF3COO)3·nH2O at temperatures up to 1,000 °C, under flowing pure Ar, O2 and O2 saturated with water vapour, was extensively analysed. The formation of HF is observed directly and the existence of a :CF2 diradical is inferred during a trifluoroacetic acid salt decomposition. High resolution thermogravimetry, differential scanning calorimetry, X-ray diffractometry and scanning electron microscopy indicated that the exothermic one-stage decomposition of the anhydrate salt occurs at 267 °C, forming YF3. Fourier transform infrared spectroscopy identified (CF3CO)2O, CF3COF, COF2, CO2 and CO as the principal volatile species; and revealed the influence of water on the reactions liberating gaseous CF3COOH, CHF3, HF, and SiF4 (from reactions with glass or quartz components). NO2 and N2O evolution suggested that traces of CH3NO2 were present in the starting material. Thermogravimetry and X-ray diffractometry indicated that the slow hydrolysis of the fluoride occurs between 630 and 655 °C, forming a mixture of Y2O3, YOF, Y7O6F9, and YF3. The decomposition and hydrolysis temperatures are significantly lower than previously reported, which has implications for sol–gel processing.

Keywords

Yttrium trifluoroacetate Yttrium oxide Yttrium oxyfluoride Yttrium fluoride HR-TG FT-IR DSC 

Notes

Acknowledgements

Mariusz Mosiadz would like to thank Mr. Robert Cornell (Polymer Characterisation Laboratory, Department of Materials Science and Metallurgy, University of Cambridge) for help with thermal analysis. Katarzyna Juda would like to gratefully acknowledge the Socrates-Erasmus Exchange Programme of the European Commission for financial support. This research was funded by the European Commission Sixth Framework Programme (MRTN-CT-2006-035619), Marie Curie Action NESPA Project (NanoEngineered Superconductors for Power Applications).

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Copyright information

© Akadémiai Kiadó, Budapest, Hungary 2011

Authors and Affiliations

  • M. Mosiadz
    • 1
  • K. L. Juda
    • 1
    • 2
  • S. C. Hopkins
    • 1
  • J. Soloducho
    • 2
  • B. A. Glowacki
    • 1
    • 3
  1. 1.Department of Materials Science and MetallurgyUniversity of CambridgeCambridgeUnited Kingdom
  2. 2.Department of ChemistryWroclaw University of TechnologyWroclawPoland
  3. 3.Institute of Power EngineeringWarsawPoland

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