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Time-resolved DXAFS study on the reduction processes of Cu cations in ZSM-5

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Abstract

The time-resolved reduction process of copper cations in/on ZSM-5 during temperature-programmed reduction (300–700 K) was studied by energy-dispersive X-ray absorption fine structure (DXAFS) as well as transmission electron microscopy (TEM). Two Cu-ZSM-5 samples with different Cu loadings were prepared by an ion-exchange method. The Cu K-edge DXAFS spectra for isolated Cu2+ species in the channels of ZSM-5 and CuO particles on the outer surfaces of ZSM-5 were recorded at an interval of 1 s during the reduction. The curve fitting analysis of the EXAFS data and the XANES analysis revealed that the isolated Cu2+ species in the channels were reduced stepwise. They were reduced to isolated Cu+ species at 400–450 K and the Cu+ species to Cu0 metallic clusters at 550–650 K. Small clusters like Cu4 were initially formed, followed by particle growth. A small part of them went out to the outer surfaces of ZSM-5 during the reduction. In contrast, CuO particles on the outer surfaces were reduced directly to Cu0 metallic particles around 450 K.

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References

  1. D.C. Koningsberger and R. Prins, eds., X-ray Absorption. Principles, Applications, Techniques of EXAFS, SEXAFS and XANES (Wiley, New York, 1988).

    Google Scholar 

  2. Y. Iwasawa, ed., X-ray Absorption Fine Structure for Catalysts and Surfaces (World Scientific, Singapore, 1996).

    Google Scholar 

  3. T. Matsushita and R.P. Phizackerley, Jpn. J. Appl. Phys. 20 (1981) 2223.

    Google Scholar 

  4. A.M. Flank, A. Fontaine, A. Jucha, M. Lemonnier, D. Raoux and C. Williams, Nucl. Instrum. Meth. 208 (1983) 651.

    Google Scholar 

  5. E. Dartyge, A. Fontaine, A. Jucha and D. Sayers, EXAFS and Near Edge Structure III (Springer, Berlin, 1984) p. 472.

    Google Scholar 

  6. E. Dartyge, A. Fontaine, G. Tourillon, R. Cortes and A. Jucha, Phys. Lett. 113 (1986) 384.

    Google Scholar 

  7. M. Hagelstein, S. Cunis, R. Frahm, W. Niemann and P. Rabe, Phys. B 158 (1989) 324.

    Google Scholar 

  8. T. Ressler, M. Hagelstein, U. Hatje and W. Metz, J. Phys. Chem. B 101 (1997) 6680.

    Google Scholar 

  9. G. Sankar, J.M. Thomas, D. Waller, J.W. Couves, C.R.A. Catlow and G.N. Greaves, J. Phys. Chem. 96 (1992) 7485.

    Google Scholar 

  10. S.G. Fiddy, M.A. Newton, A.J. Dent, G. Salvini, J.M. Corker, S. Turin, T. Campbell and J. Evans, J. Chem. Soc. Chem. Commun. 7 (1999) 851.

    Google Scholar 

  11. M. Iwamoto, H. Furukawa, Y. Mine, F. Uemura, S. Mikuriya and S. Kagawa, J. Chem. Soc. Chem. Commun. (1986) 1272.

  12. M. Iwamoto, H. Yahiro, K. Tanda, N. Mizuno, Y. Mine and S. Kagawa, J. Phys. Chem. 95 (1991) 3727.

    Google Scholar 

  13. M. Iwamoto, H. Yahiro, N. Mizuno, W.-X. Zhang, Y. Mine, H. Furukawa and S. Kagawa, J. Phys. Chem. 96 (1992) 9360.

    Google Scholar 

  14. M. Shelef, Chem. Rev. 95 (1995) 209.

    Google Scholar 

  15. V.I. Parvulescu, P. Grange and B. Delmon, Catal. Today 46 (1998) 233.

    Google Scholar 

  16. T. Beutel, J. Sarkany, G.D. Lei, J.Y. Yan and W.M.H. Sachtler, J. Phys. Chem. 100 (1996) 845.

    Article  Google Scholar 

  17. J. Sarkany, J.L. d'Itri and W.M.H. Sachtler, Catal. Lett. 16 (1992) 241.

    Google Scholar 

  18. M. Newville, P. Livins, Y. Yacoby, E.A. Stern and J.J. Rehr, Phys. Rev. B 47 (1993) 14126.

    Google Scholar 

  19. A.L. Ankudinov, B. Ravel, J.J. Rehr and S.D. Conradson, Phys. Rev. B 58 (1998) 7565.

    Google Scholar 

  20. G.G. Li, F. Bridges and C.H. Booth, Phys. Rev. B 52 (1995) 6332.

    Google Scholar 

  21. E.A. Stern, Phys. Rev. B 48 (1993) 9825.

    Google Scholar 

  22. H. Yamashita, M. Matsuoka, Y. Shioya, M. Anpo and M. Che, J. Phys. Chem. 100 (1996) 397.

    Google Scholar 

  23. T. Shido, M. Lok and R. Prins, Topics Catal. 8 (1999) 223.

    Google Scholar 

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Yamaguchi, A., Shido, T., Inada, Y. et al. Time-resolved DXAFS study on the reduction processes of Cu cations in ZSM-5. Catalysis Letters 68, 139–145 (2000). https://doi.org/10.1023/A:1019020528353

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