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Electrolytic deposits are widely used in electrochemistry and electrocatalysis. Investigation of the real structure of electrolytic deposits is of great importance as they usually posses high defectiveness that could be the reason of unusual electrocatalytic properties. The example of the exhibition of structural effects in electrocatalysis could be the dependence of the activity of Pt and Pd electrolytic deposits on the deposition potential. High-precision X-ray diffraction studies of Pt and Pd electrolytic deposits on various supports (Pt/Pt, Pd/Pt, Pt/Au) obtained at different deposition potentials were performed. The effect of the deposition potential on the structure of the deposit has been evaluated. It was shown that electrodeposited Pt and Pd have the particle size in the range from eight to twenty five nm. For the Pt electrolytic deposits systematic decrease of the Pt particle size and an increase of the concentration of the grain boundaries with the deposition potential have been found. For Pt/Pt and Pd/Pt the deposition potential influences the texture of the deposit: an increase of the deposition potential leads to the formation of more textured deposit. A decrease of the lattice parameter of nanocrystalline Pt and Pd in comparison with the value for bulk metals has been found to be the common characteristic of the electrolytic deposits. For Pt/Au systematic decrease of the Pt lattice parameter with deposition potential was observed. Thus the deposition potential is really an important variable, which could determine the structure of electrolytic deposits. The work was supported by the RFBR.

X-ray diffraction study of Pt and Pd electrolytic deposits on polycrystalline supports