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Disperse Electrolytic Platinum and Palladium Deposits of Submicron Thickness on Polycrystalline Supports: An X-ray Diffractometry and Microscopy Study

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Abstract

The structure of model electrode materials broadly used in electrocatalysis (platinized platinum, palladized platinum, platinized gold) is studied by x-ray diffractometry, scanning electron microscopy, and transmission electron microscopy. Disperse platinum and palladium coatings less than 1 μm thick are obtained by potentiostatic or galvanostatic deposition from solutions of complex chloride salts. Lattice parameters of disperse metals are shown to be considerably smaller than those of bulky crystals. Some new tendencies of variations in structural parameters with the deposition potential are revealed. Special attention is paid to a reliable determination of the size of regions of coherent scattering (ROCS) and microdistortion; in connection with this, results of approximation of reflections by various functions and a harmonic analysis of reflections are compared. The latter are used for constructing ROCS distributions by size. Good agreement is found with the STM data for platinum deposits obtained earlier. Conversely, in the case of palladium deposits, ROCS are smaller than the particle size in an outer layer of the deposit by the STM data. This result is interpreted in terms of strong concrescence of palladium nanoparticles. To determine the true surface areas of deposits and estimate continuousness of covering the support by the deposit and regularities of platinum aging on gold in conditions of potential cycling, a voltammetry method is applied.

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Authors and Affiliations

  1. Omsk Branch, Siberian Division, Russian Academy of Sciences, Boreskov Institute of Catalysis, ul. Neftezavodskaya 54, Omsk, 644053, Russia

    L. M. Plyasova, I. Yu. Molina, S. V. Cherepanova, N. A. Rudina, O. V. Sherstyuk & E. R. Savinova

  2. Moscow State University, Vorob'evy gory, Moscow, 119899, Russia

    S. N. Pron'kin & G. A. Tsirlina

Authors
  1. L. M. Plyasova
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  2. I. Yu. Molina
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  3. S. V. Cherepanova
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  4. N. A. Rudina
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  5. O. V. Sherstyuk
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  6. E. R. Savinova
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  7. S. N. Pron'kin
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  8. G. A. Tsirlina
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Plyasova, L.M., Molina, I.Y., Cherepanova, S.V. et al. Disperse Electrolytic Platinum and Palladium Deposits of Submicron Thickness on Polycrystalline Supports: An X-ray Diffractometry and Microscopy Study. Russian Journal of Electrochemistry 38, 1116–1131 (2002). https://doi.org/10.1023/A:1020607904477

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