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Agglomeration and Cleaning of Carbon Supported Palladium Nanoparticles in Electrochemical Environment

Electrocatalysis volume 5, pages 204–212 (2014)Cite this article

Abstract

Here we investigate the electrochemical behavior of Pd/C synthesized by reduction with ethylene glycol in the presence of polyvinylpyrrolidone (EG-PVP). EG-PVP produces nanoparticles (NPs) with a narrow size distribution, but some of them remain covered by impurities after the synthesis. After successive voltammetric cycles, NPs become cleaner, but some agglomeration and structural modification occur; these effects affect the electrochemical behavior of Pd/C in different ways, so we used CO as a probe to better understand the processes taking place. CO stripping shows that the general features of the multiple oxidation peaks change with the number of cycles. Possibly, CO and OH from different NPs react when the particles agglomerate, contributing to CO stripping changes. Finally, different active areas are found when the charges involved in CO oxidation and PdO reduction are compared. Such differences are rationalized in terms of a balance between the increase of sites which promote the oxidation of CO and the loss of area provoked by the growing of the particles.

After successive voltammetric cycles, Pd/C NPs become cleaner with slightly agglomeration, which lead to increase of the electrochemically active surface area. The value of area reaches a maximum, after this point the agglomeration is the main effect and contributes to the surface area decay. The agglomeration facilitates the CO electrooxidation reaction among NPs

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Acknowledgments

The authors acknowledge financial assistance from Consejo Nacional de Investigaciones Científicas y Técnicas (CONICET), UNLP, CNPq (grant # 554591/2010-3), FUNDECT (grants # 23/200.065/2008 and # 23/200.583/2012), CAPES, MINCyT, and FINEP. P.S. Fernández thanks CONICET for a fellowship. C.A. Martins thanks CNPq for a fellowship (grant # 140426/2011-6). Authors want to thank Alejandra Floridia for taking HR-TEM images.

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Authors and Affiliations

  1. Institute of Chemistry, Universidade Federal de Mato Grosso do Sul, P.O. Box 549, 79070-900, Campo Grande, Mato Grosso do Sul, Brazil

    Cauê A. Martins & Giuseppe A. Camara

  2. Instituto de Investigaciones Fisicoquímicas Teóricas y Aplicadas (INIFTA), Facultad de Ciencias Exactas, CONICET, CCT La Plata, UNLP, 1900, La Plata, Argentina

    Pablo S. Fernández & Maria E. Martins

  3. División Metales, Centro Atómico Bariloche, Av. Ezequiel Bustillo 9500, San Carlos de Bariloche, 8400, Río Negro, Argentina

    Horacio E. Troiani

  4. Department of Energy and Environment, Instituto Nacional del Carbón, CSIC, Apartado 73, 33080, Oviedo, Spain

    Ana Arenillas

Authors
  1. Cauê A. Martins
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  2. Pablo S. Fernández
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  3. Horacio E. Troiani
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  4. Maria E. Martins
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  5. Ana Arenillas
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  6. Giuseppe A. Camara
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Corresponding authors

Correspondence to Cauê A. Martins or Giuseppe A. Camara.

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Martins, C.A., Fernández, P.S., Troiani, H.E. et al. Agglomeration and Cleaning of Carbon Supported Palladium Nanoparticles in Electrochemical Environment. Electrocatalysis 5, 204–212 (2014). https://doi.org/10.1007/s12678-014-0184-3

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  • DOI: https://doi.org/10.1007/s12678-014-0184-3

Keywords

  • Palladium nanoparticles
  • PVP
  • Cleaning process
  • Agglomeration of nanoparticles
  • Active surface area
  • CO probe