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X-ray diffraction and x-ray photoelectron spectroscopy study of the Ru–Cu/SiO2 system prepared by low temperature reduction: Occurrence of a metastable amorphous or nanocrystalline phase

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Abstract

Bimetallic copper-ruthenium catalysts supported on silica were prepared by the reduction of the metallic salts in aqueous solution at room temperature. The concentration of the two metal components was selected to span the entire range of composition. In spite of the known immiscibility for the copper-ruthenium equilibrium phase diagram, X-Ray Diffraction (XRD) measurements combined with X-ray Photoelectron Spectroscopy (XPS) data indicate that this method of preparation is able to produce nanocrystalline extended solid solutions and/or amorphous metastable phases. In the case of ruthenium-rich compositions, the hexagonal close-packed (hcp) ruthenium crystallites are covered by copper atoms which grow with the same hcp sequence of the ruthenium core. For intermediate compositions a nanocrystalline and/or amorphous phase is observed, while in the case of copper-rich samples a single-phase fcc extended solid solution is found. The surface composition of the samples appears systematically enriched with Cu, as obtained from XPS semiquantitative results. The phenomena of phase separation and growth induced by thermal annealing at 870 K are also presented and discussed.

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References

  1. (a) Solid State Powder Processing, edited by A. H. Clauer and J. J. de Barbadillo (The Minerals, Metals and Materials Society, Warrendale, PA, 1990); (b) Highly Dispersed Metals, W. Romanowski, Horwood, Ltd. (John Wiley, New York, 1987).

  2. S. Davis and K. J. Klabunde, Chem. Rev. 82, 153 (1982).

    Article  CAS  Google Scholar 

  3. Transformation of Organometallics into Common and Exotic Materials: Design and Activation, edited by R. M. Laine, NATO ASI Series No. 141 (M. Nijhoff Pub., Dordrecht, 1988).

  4. (a) R. C. Wade, J. Mol. Catal. 18, 273 (1983); (b) R. C. Wade, in Speciality Inorganic Chemicals, edited by R. Thompson (The Royal Society, London, 1981), p. 25.

    Article  CAS  Google Scholar 

  5. (a) P. J. Henry, Met. Finish. 10, 45 (1984); (b) B. Ganem and J. O. Osby, Chem. Rev. 86, 763 (1986).

    Google Scholar 

  6. (a) J. O. Osby, S. W. Heinzman, and B. Ganem, J. Am. Chem. Soc. 108, 67 (1986); (b) Y. Lin Lo and B. Joe Hwang, Ind. Eng. Chem. Res. 33, 56 (1994).

    Article  CAS  Google Scholar 

  7. (a) A. Corrias, G. Ennas, G. Licheri, G. Marongiu, and G. Paschina, Chem. Mater. 2, 363 (1990); (b) G. Carturan, S. Enzo, R. Ganzerla, M. Lenarda, and R. Zanoni, J. Chem. Soc. Faraday Trans. 86, 739 (1990); (c) G. N. Glavve, K. J. Klabunde, C. M. Sorensen, and G. C. Hadjipanayis, Langmuir 9, 162 (1993); (d) A. Corrias, G. Ennas, A. Musinu, G. Marongiu, and G. Paschina, Chem. Mater. 5, 1722 (1993).

    Article  CAS  Google Scholar 

  8. (a) H. C. Brown and C. A. Brown, J. Am. Chem. Soc. 84, 1493 (1962); (b) H. C. Brown and C. A. Brown, J. Am. Chem. Soc. 84, 2827 (1962).

    Article  CAS  Google Scholar 

  9. R. C. Wade, in Catalysis of Organic Reactions, edited by W. R. Moser (Marcel Dekker, New York, 1981), p. 165.

    Google Scholar 

  10. W. Palczewska, M. Cretti-Bujnowska, J. Pielaszek, J. Sobczak, and J. Stachurski, in Proc. 9th Int. Congr. Catal. Calgary, 1988, edited by K. J. Phillips and M. Ternan (The Chemical Society of Canada, Ottawa, Ontario 1988), pp. 1410–1417.

    Google Scholar 

  11. C. Wang and C. H. Bartholomew, Appl. Catal. 62, 221 (1990).

    Article  CAS  Google Scholar 

  12. (a) M. Lenarda, R. Ganzerla, L. Storaro, and R. Zanoni, J. Mol. Cat. 78, 339 (1993); (b) M. Lenarda, R. Ganzerla, L. Storaro, and R. Zanoni, J. Mol. Cat. 79, 243 (1993).

    Article  CAS  Google Scholar 

  13. J. van Wonterghem, S. Morup, C. J. W. Koch, S. W. Charles, and S. Wells, Nature (London) 322, 622 (1986).

    Article  CAS  Google Scholar 

  14. A. L. Oppengard, F. J. Darnell, and H. C. Miller, J. Appl. Phys. 32, suppl. 3, 184s (1961).

    Article  Google Scholar 

  15. J. H. Sinfelt, J. Catal. 29, 308 (1973).

    Article  CAS  Google Scholar 

  16. J. H. Sinfelt, Acc. Chem. Res. 10, 15 (1977).

    Article  CAS  Google Scholar 

  17. J. H. Sinfelt, Rev. Mod. Phys. 51, 569 (1979).

    Article  CAS  Google Scholar 

  18. J. K. A. Clarke, Chem. Rev. 75, 291 (1975).

    Article  CAS  Google Scholar 

  19. J. K. A. Clarke and A. C. M. Creaner, Ind. Eng. Chem. Prod. Res. Dev. 20, 574 (1981).

    Article  CAS  Google Scholar 

  20. M. Hansen and K. Anderko, Constitution of Binary Alloys, 2nd ed. (McGraw-Hill, New York, 1958).

    Google Scholar 

  21. G. C. Bond and B. D. Turnham, J. Catal. 45, 128 (1976).

    Article  CAS  Google Scholar 

  22. J. H. Sinfelt, Y. L. Lam, J. A. Cusumano, and A. E. Barnett, J. Catal. 42, 227 (1976).

    Article  CAS  Google Scholar 

  23. E. B. Prestridge, G. H. Via, and J. H. Sinfelt, J. Catal. 50, 115 (1977).

    Article  CAS  Google Scholar 

  24. J. H. Sinfelt, G. H. Via, and F. W. Lytle, J. Chem. Phys. 72, 4832 (1980).

    Article  CAS  Google Scholar 

  25. A. J. Rouco, G. L. Haller, J. A. Oliver, and C. Kemball, J. Catal. 84, 297 (1983).

    Article  CAS  Google Scholar 

  26. G. L. Haller, D. E. Resasco, and J. Wang, J. Catal. 84, 477 (1983).

    Article  CAS  Google Scholar 

  27. S. Y. Lai and J. C. Vicherman, J. Catal. 90, 337 (1984).

    Article  CAS  Google Scholar 

  28. G. C. Bond and X. Yide, J. Mol. Catal. 25, 141 (1984).

    Article  CAS  Google Scholar 

  29. X. Guo, Q. Xin, Y. Li, D. Jin, and P. Ying, in Proceedings 8th International Congress on Catalysis, Berlin, 1984 (Dechema, Frankfurt-am-Main, Germany, 1984), Vol. IV, p. 599.

    Google Scholar 

  30. A. G. Shastri, J. Schwank, and S. Galvagno, J. Catal. 100, 446 (1986).

    Article  CAS  Google Scholar 

  31. D. E. Damiani, E. D. Perez Millan, and A. J. Rouco, J. Catal. 101, 162 (1986).

    Article  CAS  Google Scholar 

  32. M. C. Schoenmaker-Stoil, J. W. Verwijs, and J. J.F. Scholten, Appl. Catal. 30, 339 (1987).

    Article  Google Scholar 

  33. A. J. Hong, A. J. Rouco, D. E. Resasco, and G. L. Haller, J. Phys. Chem. 91, 2665 (1987).

    Article  CAS  Google Scholar 

  34. A. J. Hong, B. J. McHugh, L. Bonneviot, D. E. Resasco, R. S. Weber, and G. L. Haller, in Proceedings 9th International Congress on Catalysis, edited by M. J. Phillip and M. Ternan, Calgary, 1988 (Chemical Institute of Canada, Ottawa 1988), Vol. 3, p. 1198.

    Google Scholar 

  35. J. H. Sinfelt, Int. Rev. Phys. Chem. 7, 281 (1988).

    Article  Google Scholar 

  36. C. Crisafulli, R. Maggiore, G. Schembari, S. Sciré, and S. Galvagno, J. Mol. Catal. 50, 67 (1989).

    Article  CAS  Google Scholar 

  37. Rembiao Liu, B. Tesche, and H. Knoezinger, J. Catal. 129, 402 (1991).

    Article  CAS  Google Scholar 

  38. M. W. Smale and T. S. King, J. Catal. 120, 335 (1990).

    Article  Google Scholar 

  39. M. Sprock, X. Wu, and T. S. King, J. Catal. 138, 617 (1992).

    Article  CAS  Google Scholar 

  40. C. Crisafulli, R. Maggiore, S. Sciré, L. Solarino, and S. Galvagno, J. Mol. Catal. 63, 55 (1990).

    Article  CAS  Google Scholar 

  41. X. Wu, B. C. Gerstein, and T. S. King, J. Catal. 121, 271 (1990).

    Article  CAS  Google Scholar 

  42. X. Wu, S. Bathia, and T. S. King, J. Vac. Sci. Technol. A 10 (4), 2729 (1992).

    Article  CAS  Google Scholar 

  43. C. Crisafulli, R. Maggiore, S. Sciré, S. Galvagno, and C. Milone, J. Mol. Catal. 83, 237 (1993).

    Article  CAS  Google Scholar 

  44. (a) K. Uenishi, K. F. Kobayashi, S. Nasu, H. Hatano, K. N. Ishibara, and P. H. Shingu, Z. Metallk. 83, 2 (1992); (b) P. P. Macrì, P. Rose, R. Frattini, S. Enzo, G. Principi, W. X. Hu, and N. Cowlam, J. Appl. Phys. 76, 4061 (1994).

    Google Scholar 

  45. G. Cocco, S. Enzo, L. Schiffini, and L. Battezzati, in New Materials by Mechanical Alloying Techniques, edited by E. Artz and L. Schultz (Deutsche Gessellschaft fur Metallkunde, Oberursel, Germany, 1989), p. 279.

    Google Scholar 

  46. A. Van Neste, A. Lamarre, M. L. Trudeau, and R. Schulz, J. Mater. Res. 7, 2412 (1992).

    Article  Google Scholar 

  47. Practical Surface Analysis, 2nd ed., D. Briggs and M. P. Seah (John Wiley & Sons Ltd. Chichester, U.K., 1990), Vol. 1, appendix 4, p. 587.

  48. N. S. McIntyre and M. G. Cook, Anal. Chem. 47, 2208 (1975).

    Article  Google Scholar 

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Authors and Affiliations

  1. Department of Chemistry, University of Venice “Ca’Foscari”, Calle Larga S. Marta 2137, 30123, Venice, Italy

    Maurizio Lenarda, Renzo Ganzerla & Loretta Storaro

  2. Department of Physical Chemistry, University of Venice “Ca’Foscari”, Calle Larga S. Marta 2137, 30123, Venice, Italy

    Romana Frattini

  3. Department of Chemistry, University of Sassari, via Vienna 2, 07100, Sassari, Italy

    Stefano Enzo

  4. Department of Chemistry, University of Rome “La Sapienza”, Piazzale A. Moro 5, 00185, Rome, Italy

    Roberto Zanoni

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  1. Maurizio Lenarda
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  2. Renzo Ganzerla
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  3. Loretta Storaro
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  4. Romana Frattini
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  5. Stefano Enzo
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  6. Roberto Zanoni
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Lenarda, M., Ganzerla, R., Storaro, L. et al. X-ray diffraction and x-ray photoelectron spectroscopy study of the Ru–Cu/SiO2 system prepared by low temperature reduction: Occurrence of a metastable amorphous or nanocrystalline phase. Journal of Materials Research 11, 325–331 (1996). https://doi.org/10.1557/JMR.1996.0038

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