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Abstract <p>The thermal decomposition of copper(II) oxalate CuC<sub>2</sub>O<sub>4</sub>⋅0.5H<sub>2</sub>O and potassium oxalatocuprate(II) K<sub>2</sub>Cu(C<sub>2</sub>O<sub>4</sub>)<sub>2</sub>⋅2H<sub>2</sub>O in vacuum at a residual pressure of 10<sup>–5</sup> Torr has been studied in the range from room temperature to 400°C with operando recording the X-ray photoelectron (XPS) and Auger spectra. An&#xa0;X-ray photoelectron spectrometer with a magnetic energy analyzer was used. An analysis of the XP and Auger spectroscopy data shows that the thermal decomposition of CuC<sub>2</sub>O<sub>4</sub>⋅0.5H<sub>2</sub>O includes the following stages: elimination of crystallization water (150–265°C); elimination of CO<sub>2</sub> (265–285°C), forming an unstable intermediate product; and decomposition of the latter at 285°C, forming a residue of metallic copper with an admixture of 11–13 mol&#xa0;% copper(I) oxide. The thermal decomposition of K<sub>2</sub>Cu(C<sub>2</sub>O<sub>4</sub>)<sub>2</sub>⋅2H<sub>2</sub>O includes the stages of elimination of crystallization water (85–120°C) and decomposition of the resulting anhydrous oxalate with elimination of CO<sub>2</sub>&#xa0;and CO (250–290°C).</p>

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Thermal Decomposition of Copper Oxalate and Potassium Oxalatocuprate: Operando XPS Study

  • 期刊论文

  • 发表日期：

    2025年4月25日

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  • N. V. Lomova,
  • I. S. Kazantseva,
  • M. A. Shumilova,
  • N. N. Pastukhova,
  • N. Yu. Isupov,
  • D. S. Rybin,
  • F. F. Chausov,
  • V. V. Boldyrev

摘要

Abstract

The thermal decomposition of copper(II) oxalate CuC2O4⋅0.5H2O and potassium oxalatocuprate(II) K2Cu(C2O4)2⋅2H2O in vacuum at a residual pressure of 10–5 Torr has been studied in the range from room temperature to 400°C with operando recording the X-ray photoelectron (XPS) and Auger spectra. An X-ray photoelectron spectrometer with a magnetic energy analyzer was used. An analysis of the XP and Auger spectroscopy data shows that the thermal decomposition of CuC2O4⋅0.5H2O includes the following stages: elimination of crystallization water (150–265°C); elimination of CO2 (265–285°C), forming an unstable intermediate product; and decomposition of the latter at 285°C, forming a residue of metallic copper with an admixture of 11–13 mol % copper(I) oxide. The thermal decomposition of K2Cu(C2O4)2⋅2H2O includes the stages of elimination of crystallization water (85–120°C) and decomposition of the resulting anhydrous oxalate with elimination of CO2 and CO (250–290°C).