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Combining XRD and EXAFS with on-Line Catalytic Studies for in situ Characterization of Catalysts

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Abstract

Advances in the study of catalysts by in situ structural characterization, using X-ray absorption spectroscopy (XAFS) and X-ray diffraction (XRD), have recently been achieved and they are illustrated by reference to several examples. Emphasis in the present overview is laid on the study of catalysts under realistic working conditions and therefore in particular on-line gas analysis during activation and/or during catalysis. The examples encompass (a) activation of copper-based methanol catalysts, (b) dynamic changes of copper-based catalysts during methanol synthesis conditions, (c) catalytic partial oxidation on Rh/Al2O3 catalysts, and (d) reduction (activation) of copper-promoted high temperature shift catalysts.

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References

  1. R. Burch, ed., Insitu Methods in Catalysis, Catal. Today 9 (1991).

  2. B.S. Clausen, L. Gråbæk, G. Steffensen, P.L. Hansen and H. Topsøe, Catal. Lett. 20 (1993) 23.

    Google Scholar 

  3. J.W. Niemantsverdriet, Spectroscopy in Catalysis (VCH, Weinheim, 1993).

    Google Scholar 

  4. B.S. Clausen, H. Topsøe and R. Frahm, Adv. Catal. 42 (1998) 315.

    Google Scholar 

  5. R. Prins and D.C. Koningsberger, eds., in: X-ray Absorption: Principles, Applications, Techniques of EXAFS, SEXAFS and XANES (Wiley, New York, 1988) p. 321.

    Google Scholar 

  6. H. Topsøe, Stud. Surf. Sci. Catal. 130 (2000) 1.

    Google Scholar 

  7. B.S. Clausen and H. Topsøe, Catal. Today 9 (1991) 189.

    Google Scholar 

  8. B.S. Clausen, G. Steffensen, B. Fabius, J. Villadsen, R. Feidenhans'l and H. Topsøe, J. Catal. 132 (1991) 524.

    Google Scholar 

  9. J.W. Couves, J.M. Thomas, D. Waller, R.H. Jones, A.J. Dent, G.E. Derbyshire and G.N. Greaves, Nature 354 (1991) 465.

    Google Scholar 

  10. T. Matsushita and U. Kaminaga, Jpn. J. Appl. Cryst. 13 (1980).

  11. M. Hagelstein, S. Cunis, R. Frahm, W. Nieman and P. Rabe, Physica B 158 (1989) 324.

    Google Scholar 

  12. M. Hagelstein, C. Ferrero, U. Hatje, T. Ressler and W. Metz, J. Synchr. Rad. 2 (1995) 174.

    Google Scholar 

  13. R. Frahm, Physica B 158 (1989) 342.

    Google Scholar 

  14. R. Frahm, Rev. Sci. Instrum. 60 (1989) 2515.

    Google Scholar 

  15. R. Frahm, J. Weigelt, G. Meyer and G. Materlik, Rev. Sci. Instrum. 66 (1995) 1677.

    Google Scholar 

  16. H. Bornebusch, B.S. Clausen, G. Steffensen, D. Lützenkirchen-Hecht and R. Frahm, J. Synchr. Rad. 6 (1999) 209.

    Google Scholar 

  17. S. Pascarelli, T. Neisius and S. DePanfilis, J. Synchr. Rad. 6 (1999) 1044.

    Google Scholar 

  18. S. Rashid and X. Turrillas, Thermochim. Acta 302 (1997) 25.

    Google Scholar 

  19. V. Gauthier, F. Bernard, E. Gaffet, C. Josse and J.P. Larpin, Mater. Sci. Eng. A 272 (1999) 334.

    Google Scholar 

  20. J.-D. Grunwaldt, A.M. Molenbroek, N.-Y. Topsøe, H. Topsøe and B.S. Clausen, J. Catal. 194 (2000) 452.

    Google Scholar 

  21. A. Gualtieri, P. Norby, G. Artoli and J. Hanson, Micropor. Mater. 9 (1997) 189.

    Google Scholar 

  22. D. O'Hare, J.S.O. Evans, R.J. Francis, P.S. Halasyamani, P. Norby and J. Hanson, Micropor. Mesopor. Mater. 21 (1998) 253.

    Google Scholar 

  23. G. Sankar and J.M. Thomas, Topics Catal. 8 (1999) 1.

    Google Scholar 

  24. G. Sankar, J.M. Thomas and C.R.A. Catlow, Topics Catal. 10 (2000) 255.

    Google Scholar 

  25. T. Ressler, R.E. Jentoft, J. Wienold, M.M. Günter and O. Timpe, J. Phys. Chem. B 104 (2000) 6360.

    Google Scholar 

  26. T. Ressler, O. Timpe, T. Neisius, J. Find, G. Mestl, M. Dieterle and R. Schlögl, J. Catal. 191 (2000) 75.

    Google Scholar 

  27. J.S.O. Evans, R.J. Francis, D. O'Hare, S.J. Price, S.M. Clark, J. Flaherty, J. Gordon, A. Nield and C.C. Tang, Rev. Sci. Instrum. 66 (1995) 2442.

    Google Scholar 

  28. C.H. Gras, F. Charlot, E. Gaffet, F. Bernard and J.C. Biepce, Acta Mater. 47 (1999) 2113.

    Google Scholar 

  29. B.S. Clausen, Catal. Today 39 (1998) 293.

    Google Scholar 

  30. S.R. Davis, A.V. Chadwick and J.D. Wright, J. Phys. Chem. 101 (1997) 9901.

    Google Scholar 

  31. I.J. Shannon, T. Maschmeyer, G. Sankar, J.M. Thomas, R.D. Oldroyd, M. Sheehy, D. Madill, A.D. Waller and R.P. Townsend, Catal. Lett. 23 (1997) 23.

    Google Scholar 

  32. R.I. Walton, A.J. Dent and S.J. Hibble, Chem. Mater. 10 (1998) 3737.

    Google Scholar 

  33. M.M. Günter, B. Behms, R. Schlögl and T. Ressler, J. Synchr. Rad. 8 (2001) 619.

    Google Scholar 

  34. A. Yamagushi, T. Shido, Y. Inada, T. Kongure, K. Asakura, M. Nomura and Y. Iwasawa, Catal. Lett. 68 (2000) 139.

    Google Scholar 

  35. G. Sankar, J.M. Thomas, F. Rey and G.N. Greaves, J. Chem. Soc. Chem. Commun. (1995) 2549.

  36. P. Kappen, L. Tröger, H. Zink, G. Materlik, C. Reckleben, K. Hansen, J.-D. Grunwaldt and B.S. Clausen, to be published.

  37. J.-D. Grunwaldt, P. Kappen, B.S. Hammershøj, L. Tröger and B.S. Clausen, J. Synchr. Rad. 8 (2001) 572.

    Google Scholar 

  38. P. Kappen, L. Tröger, H. Zink, G. Materlik, C. Reckleben, K. Hansen, J.-D. Grunwaldt and B.S. Clausen, HASYLAB Annual Report 1998, HASYLAB, DESY, Hamburg (1999) p. 847.

    Google Scholar 

  39. B.S. Clausen and J.K. Nørskov, Topics Catal. 10 (2000) 221.

    Google Scholar 

  40. J. Als-Nielsen, G. Grübel and B.S. Clausen, Nucl. Instrum. Methods Phys. Res. B 97 (1995) 522.

    Google Scholar 

  41. J.-D. Grunwaldt, D. Lützenkirchen-Hecht, M. Richwin, S. Grundmann, B.S. Clausen and R. Frahm, J. Phys. Chem. B, in press.

  42. B.S. Clausen, B. Lengeler, B.S. Rasmussen, W. Niemann and H. Topsøe, J. Phys. (Paris) C8 (1986) 237.

  43. B.S. Clausen, J. Schiøtz, L. Gråbek, C.V. Ovesen, K.W. Jacobsen, J.K. Nørskov and H. Topsøe, Topics Catal. 1 (1994) 367.

    Google Scholar 

  44. C.V. Ovesen, B.S. Clausen, J. Schiøtz, P. Stoltze, H. Topsøe and J.K. Nørskov, J. Catal. 168 (1997) 133.

    Google Scholar 

  45. N.-Y. Topsøe and H. Topsøe, Topics Catal. 8 (1999) 267.

    Google Scholar 

  46. N.-Y. Topsøe and H. Topsøe, J. Mol. Catal. 141 (1999) 95.

    Google Scholar 

  47. E.K. Poels and D.S. Brands, Appl. Catal. A 191 (2000) 83.

    Google Scholar 

  48. T.M. Yurieva, L.M. Plyasova, O.V. Makarova and T.A. Krieger, J. Mol. Catal. A 113 (1996) 455.

    Google Scholar 

  49. I. Böttger, T. Schedel-Niedrig, O. Timpe, R. Gotschall, M. Hävecker, T. Ressler and R. Schlögl, Chem. Eur. J. 6 (2000) 1870.

    Google Scholar 

  50. H. Topsøe, C.V. Ovesen, B.S. Clausen, N.-Y. Yopsøe, P.E.H. Nielsen, E. Törnqvist and J.K. Nørskov, in: Dynamics of Surfaces and Reaction Kinetics in Heterogeneous Catalysis (Elsevier, 1997) p. 121.

  51. J.-D. Grunwaldt, L. Basini, A. Kjersgaard, G. Steffensen and B.S. Clausen, HASYLAB Annual Report 1998, HASYLAB, DESY, Hamburg (1999) p. 827.

    Google Scholar 

  52. J.-D. Grunwaldt, L. Basini and B.S. Clausen, J. Catal., in press.

  53. L. Basini, M. Marchionna and A. Aragno, J. Phys. Chem. 96 (1992) 9431.

    Google Scholar 

  54. H.F. van't Blik, J.B.A.D. van Zon, T. Huizinga, J.C. Vis, D.C. Koningsberger and R. Prins, J. Phys. Chem. 87 (1983) 2264.

    Google Scholar 

  55. H.F.J. van't Blik, J.B.A. van Zon, T. Huiziga, J.C. Vis, D.C. Koningsberger and R. Prins, J. Am. Soc. 107 (1985) 3139.

    Google Scholar 

  56. T. Mizushima, K. Tohij, Y. Udagawa and A. Ueno, J. Am. Chem. Soc. 112 (1990) 7887.

    Google Scholar 

  57. L. Basini, A. Guarinoni and K. Aasberg-Petersen, Stud. Surf. Sci. Catal. 119 (1998) 699.

    Google Scholar 

  58. L. Basini, A. Guarinoni and A. Aragno, J. Catal. 190 (2000) 284.

    Google Scholar 

  59. J. Jaklevic, J.A. Kirby, M.P. Klein, A.S. Robertson, G.S. Brown and P. Eisenberger, Solid State Commun. 23 (1977) 679.

    Google Scholar 

  60. F.W. Lytle, R.B. Greegor, D.R. Sandstrom, E.C. Marques, J. Wong, C.L. Spiro, G.P. Huffman and F.E. Huggins, Nucl. Instrum. Methods Phys. Res. 226 (1984) 542.

    Google Scholar 

  61. P. Kappen, J.-D. Grunwaldt, B.S. Hammershøi, L. Tröger and B.S. Clausen, J. Catal. 198 (2001) 56.

    Google Scholar 

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Grunwaldt, JD., Clausen, B.S. Combining XRD and EXAFS with on-Line Catalytic Studies for in situ Characterization of Catalysts. Topics in Catalysis 18, 37–43 (2002). https://doi.org/10.1023/A:1013838428305

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