<p>The composition and oxidation state of metals in copper amalgam samples obtained by the direct reduction of copper and mercury ions in an aqueous solution were studied by x-ray photoelectron spectroscopy (XPS) in an atmosphere of high-purity argon 6.0. The use of XPS in a high-purity argon medium eliminates the effect of oxygen traces in the residual atmosphere of the spectrometer on the amalgam surface and the investigation results. The order of the reduction of the metal ions in an aqueous formaldehyde solution was shown to affect the content of oxidized copper forms. In the case of simultaneous reduction of copper and mercury ions, the amalgam obtained had an impurity of 5–7 at.% copper as cuprous oxide and 8–10 at.% copper as cupric oxide. After the consecutive reduction of copper ions followed by mercury ions, the resultant amalgam had an impurity of 11–14 at.% copper as cupric oxide. When the copper ions were reduced by washing the resultant powder with dilute acid followed by the reduction of mercury, the resultant amalgam contained an impurity of 9–11 at.% copper as cuprous oxide. The state of mercury in the amalgam was found to be independent of the order of reduction of the metal ions.</p>

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X-Ray Photoelectron Spectroscopy in a High-Purity Argon Atmosphere for Studying Functional Materials Using Copper Amalgam as an Example

  • M. Yu. Alies,
  • E. Yu. Shelkovnikov,
  • F. F. Chausov,
  • N. V. Lomova,
  • N. Yu. Isupov

摘要

The composition and oxidation state of metals in copper amalgam samples obtained by the direct reduction of copper and mercury ions in an aqueous solution were studied by x-ray photoelectron spectroscopy (XPS) in an atmosphere of high-purity argon 6.0. The use of XPS in a high-purity argon medium eliminates the effect of oxygen traces in the residual atmosphere of the spectrometer on the amalgam surface and the investigation results. The order of the reduction of the metal ions in an aqueous formaldehyde solution was shown to affect the content of oxidized copper forms. In the case of simultaneous reduction of copper and mercury ions, the amalgam obtained had an impurity of 5–7 at.% copper as cuprous oxide and 8–10 at.% copper as cupric oxide. After the consecutive reduction of copper ions followed by mercury ions, the resultant amalgam had an impurity of 11–14 at.% copper as cupric oxide. When the copper ions were reduced by washing the resultant powder with dilute acid followed by the reduction of mercury, the resultant amalgam contained an impurity of 9–11 at.% copper as cuprous oxide. The state of mercury in the amalgam was found to be independent of the order of reduction of the metal ions.