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Elucidation of the chemical state of phosphorus and boron in crystallographically amorphous nickel electroplates

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Abstract

Using the valence-to-core version of X-ray emission spectroscopy (valence-to-core XES) together with X-ray diffraction analysis, the structure and the composition of nickel coatings deposited from solutions containing hypophosphite ions or dimethylaminoborane (DMAB) are studied. The diffraction patterns of prepared deposits are characterized by the presence of a wide “halo”. Annealing of crystallographically amorphous deposits at temperatures of 500°C and higher transforms these haloes into the spectra corresponding to metal nickel and its phosphides or borides present in the crystallized deposits. A result of fundamental importance obtained in the simultaneously conducted examination of the same deposits by the valence-to-core XES method is that both the binding energy and the intensities of Kβ satellite spectral lines of annealed samples remain unchanged as compared with original samples. Based on this comparison, it is concluded that phosphide and boride nickel compounds were already formed in the course of electrodeposition, whereas the thermal treatment of deposits (crystallization) leads only to aggregation of the metal and metal-metalloid nanoparticles.

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Authors and Affiliations

  1. Swiss-Norwegian Beamlines at of the European Synchrotron Radiation Facility, Grenoble, France

    O. V. Safonova

  2. Faculty of Chemistry, Moscow State University, Vorob’evy Gory, Moscow, 119992, Russia

    L. N. Vykhodtseva, L. A. Fishgoit & V. A. Safonov

  3. Vernadskii Institute of Geochemistry and Analytical Chemistry, Russian Academy of Sciences, ul. Kosygina 19, Moscow, 119995, Russia

    N. N. Kononkova

  4. European Synchrotron Radiation Facility, Grenoble, France

    P. Glatzel

Authors
  1. O. V. Safonova
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  2. L. N. Vykhodtseva
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  3. L. A. Fishgoit
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  4. N. N. Kononkova
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  5. P. Glatzel
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  6. V. A. Safonov
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Corresponding author

Correspondence to V. A. Safonov.

Additional information

Original Russian Text © O.V. Safonova, L.N. Vykhodtseva, L.A. Fishgoit, N.N. Kononkova, P. Glatzel, V.A. Safonov, 2010, published in Elektrokhimiya, 2010, Vol. 46, No. 11, pp. 1307–1314.

The paper was prepared for a special issue dedicated to the birth centenary of Ya.M. Kolotyrkin.

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Safonova, O.V., Vykhodtseva, L.N., Fishgoit, L.A. et al. Elucidation of the chemical state of phosphorus and boron in crystallographically amorphous nickel electroplates. Russ J Electrochem 46, 1223–1229 (2010). https://doi.org/10.1134/S1023193510110030

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  • DOI: https://doi.org/10.1134/S1023193510110030

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