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Agglomeration and Cleaning of Carbon Supported Palladium Nanoparticles in Electrochemical Environment

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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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References

  1. M. Watanabe, S. Motoo, J. Electroanal. Chem. 60, 275 (1975)

    Article  CAS  Google Scholar 

  2. Y.C. Wei, C.W. Liu, W.D. Kang, C.M. Lai, L.D. Tsai, K.W. Wang, J. Electroanal. Chem. 660, 64 (2011)

    Article  CAS  Google Scholar 

  3. Y. Bi, L. Chen, G. Lu, J. Mol. Catal. A Chem. 266, 173 (2007)

    Article  CAS  Google Scholar 

  4. M. Chen, Y. Xing, Langmuir 21, 9334 (2005)

    Article  CAS  Google Scholar 

  5. P.S. Fernández, M.E. Martins, G.A. Camara, Electrochim. Acta 66, 180 (2012)

    Article  Google Scholar 

  6. H. Hei, H. He, R. Wang, X. Liu, G. Zhang, Soft Nanosci. Lett. 2, 34 (2012)

    CAS  Google Scholar 

  7. C. Susut, T.D. Nguyen, G.B. Chapman, Y. Tong, Electrochim. Acta 53, 6135 (2008)

    Article  CAS  Google Scholar 

  8. D. Li, C. Wang, D. Tripkovic, S. Sun, N.M. Markovic, V.R. Stamenkovic, ACS Catal. 2, 1358 (2012)

    Article  CAS  Google Scholar 

  9. A. Goel, N. Rani, Open J. Inorg. Chem. 2, 67 (2012)

    Article  Google Scholar 

  10. K. Gong, M.B. Vukmirovic, C. Ma, Y. Zhu, R.R. Adzic, J. Electroanal. Chem. 662, 213 (2011)

    Article  CAS  Google Scholar 

  11. L.H.S. Gasparotto, J.F. Gomes, G. Tremiliosi-Filho, J. Electroanal. Chem. 663, 48 (2011)

    Article  CAS  Google Scholar 

  12. A.M. Hofstead-Duffy, D.J. Chen, Y.J. Tong, Electrochim. Acta 82, 543 (2012)

    Article  CAS  Google Scholar 

  13. C. Coutanceau, P. Urchaga, S. Brimaud, S. Baranton, Electrocatal. 3, 75 (2012)

    Article  CAS  Google Scholar 

  14. J. Solla-Gullon, V. Montiel, A. Aldaz, J. Clavilier, J. Electroanal. Chem. 491, 69 (2000)

    Article  CAS  Google Scholar 

  15. P.S. Fernández, D.S. Ferreira, C.A. Martins, H.E. Troiani, G.A. Camara, M.E. Martins, Electrochim. Acta 98, 25 (2013)

    Article  Google Scholar 

  16. P.L. Redmond, A.J. Hallock, L.E. Brus, Nano Lett. 5, 131 (2005)

    Article  CAS  Google Scholar 

  17. F.R. Nikkuni, E.A. Ticianelli, L. Dubau, M. Chatenet, Electrocatal. 4, 104 (2013)

    Article  CAS  Google Scholar 

  18. O.V. Chertiouk, P.A. Simonov, E.R. Savinova, Electrochim. Acta 48, 3851 (2003)

    Article  Google Scholar 

  19. F. Maillard, E.R. Savinova, P.A. Simonov, V.I. Zaikovskii, U. Stimming, J. Phys. Chem. B 108, 17893 (2004)

    Article  CAS  Google Scholar 

  20. F. Maillard, E.R. Savinova, U. Stimming, J. Electroanal. Chem. 599, 221 (2007)

    Article  CAS  Google Scholar 

  21. G.A. Camara, J.F. Gomes, K. Bergamaski, E. Teixeira-Neto, F.C. Nart, J. Electroanal. Chem. 617, 171 (2008)

    Article  CAS  Google Scholar 

  22. A. López-Cudero, J. Solla-Gullón, E. Herrero, A. Aldaz, J.M. Feliu, J. Electroanal. Chem. 644, 117 (2010)

    Article  Google Scholar 

  23. S. Park, S.A. Waisileski, M.J. Weaver, J. Phys. Chem. B 105, 9719 (2001)

    Article  CAS  Google Scholar 

  24. S. Park, Y.J. Tong, A. Wieckowski, M.J. Weaver, Langmuir 18, 3233 (2002)

    Article  CAS  Google Scholar 

  25. R. Lamber, S. Wetjen, N.I. Jaeger, Phys. Rev. B Solid State 51, 10968 (1995)

    Article  CAS  Google Scholar 

  26. A.E. Bolzán, J. Electroanal. Chem. 380, 127 (1995)

    Article  Google Scholar 

  27. A. Marcu, G. Toth, R. Srivastava, P. Strasser, J. Power Sources 208, 288 (2012)

    Article  CAS  Google Scholar 

  28. F. Hasché, M. Oezaslan, P. Strasser, ChemCatChem 3, 1805 (2011)

    Google Scholar 

  29. F. Hasche, M. Oezaslan, P. Strasser, Phys. Chem. Chem. Phys. 12, 15251 (2010)

    Article  CAS  Google Scholar 

  30. W.J. Plieth, J. Phys. Chem. 86, 3166 (1982)

    Article  CAS  Google Scholar 

  31. L. Tang, B. Han, K. Persson, C. Friesen, T. He, K. Sieradzki, G. Ceder, J. Am. Chem. Soc. 132, 596 (2009)

    Article  Google Scholar 

  32. H.A. Kozlowska, J.O.’.M. Bockris, in Comprehensive Treatise of Electrochemistry, ed. by E.B. Yeager, B.E. Conway, S. Sarangapani, vol. 9 (Plenum, New York, 1984), p. 2

    Google Scholar 

  33. R.S. Ferreira Jr., M.J. Giz, G.A. Camara, J. Electroanal. Chem. 697, 15 (2013)

    Article  CAS  Google Scholar 

  34. Y. Sugawara, A.P. Yadav, A. Nishikata, T. Tsuru, J. Electroanal. Chem. 662, 379 (2011)

    Article  CAS  Google Scholar 

  35. K.J.J. Mayrhofer, M. Arenz, B.B. Blizanac, V. Stamenkovic, P.N. Ross, N.M. Markovic, Electrochim. Acta 50, 5144 (2005)

    Article  CAS  Google Scholar 

  36. J.S. Spendelow, J.D. Goodpaster, P.J.A. Kenis, A. Wieckowski, J. Phys. Chem. B 110, 9545 (2006)

    Article  CAS  Google Scholar 

  37. B. Hammer, O.H. Nielsen, J.K. Norskov, Catal. Lett. 46, 31 (1997)

    Article  CAS  Google Scholar 

  38. M. Arenz, K.J.J. Mayrhofer, V. Stamenkovic, B.B. Blizanac, T. Tomoyuki, P.N. Ross, N.M. Markovic, J. Am. Chem. Soc. 127, 6819 (2005)

    Article  CAS  Google Scholar 

  39. Y.S. Horn, W.C. Sheng, S. Chen, P.J. Ferreira, E.F. Holby, D. Morgan, Top. Catal. 46, 285 (2007)

    Article  Google Scholar 

  40. J. Clavilier, D. Armand, J. Electroanal. Chem. 199, 187 (1986)

    Article  CAS  Google Scholar 

  41. C. Grolleau, C. Coutanceau, F. Pierre, J.-M. Léger, Electrochim. Acta 53, 7157 (2008)

    Article  CAS  Google Scholar 

  42. Z. Cui, P.J. Kulesza, C.M. Li, W. Xing, S.P. Jiang, Int. J. Hydrogen Energy 36, 8508 (2011)

    Article  CAS  Google Scholar 

  43. C. Hsu, C. Huang, Y. Hao, F. Liu, Phys. Chem. Chem. Phys. 14, 14696 (2012)

    Article  CAS  Google Scholar 

  44. R. Lin, C. Cao, H. Zhang, H. Huang, J. Ma, Int. J. Hydrogen Energy 37, 4648 (2012)

    Article  CAS  Google Scholar 

  45. C. Hsu, C. Huang, Y. Hao, F. Liu, Electrochem. Commun. 23, 133 (2012)

    Article  CAS  Google Scholar 

  46. E. Antolini, J. Power Sources 170, 1 (2007)

    Article  CAS  Google Scholar 

  47. D.F. van der Vliet, C. Wang, D. Li, A.P. Paulikas, J. Greeley, R.B. Rankin, D. Strmcnik, D. Tripkovic, N.M. Markovic, V.R. Stamenkovic, Angew. Chem. 124, 3193 (2012)

    Article  Google Scholar 

Download references

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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