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In Situ EXAFS Characterization of Nanoparticulate Catalysts

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Abstract

X-ray absorption fine structure (XAFS) spectroscopy probes the structure and electronic properties of metal centers. Because it can be applied to noncrystalline materials, it is a key technique for probing nanoparticulate materials, such as colloidal and heterogeneous metal catalysts. The high brilliance of modern synchrotron radiation x-ray sources facilitates in situ studies, which provide direct structure–function relationships with both spatial and time resolution; this is especially effective when applied in combination with complementary techniques such as x-ray diffraction, mass spectrometry, and optical or vibrational spectroscopies. Tracking the particle formation of platinum-group metal catalysts, their behavior under reaction conditions, and the distribution of sites within a catalyst bed shows that this approach is essential for understanding the chemistry of these nanoparticles. Rather than behave as monolithic entities, nanoparticulate catalysts undergo rapid structural transformations induced by the gas environment and reaction conditions, and their lifetimes as catalysts depend on the reversibility of these changes.

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References

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

    Google Scholar 

  2. P. Brinkgreve, D.C. Koningsberger, Patent Application NL8300927 (1983).

  3. M.F. Ravet, G. Krill, Rev. Sci. Instrum. 54, 227 (1983).

    Google Scholar 

  4. A. Williams, Rev. Sci. Instrum. 54, 193 (1983).

    Article  CAS  Google Scholar 

  5. S. Yamashita, K. Taniguchi, S. Nomoto, T. Yamaguchi, H. Wakita, X-ray Spectrom. 21, 91 (1992).

    Article  CAS  Google Scholar 

  6. M. Tromp, J.A. van Bokhoven, G.P.F. van Strijdonck, P.W.N.M. van Leeuwen, D.C. Koningsberger, D.E. Ramaker, J. Am. Chem. Soc. 127, 777 (2005).

    Article  CAS  Google Scholar 

  7. M. Wilke, F. Farges, P.E. Petit, G.E. Brown, F. Martin, Am. Mineral. 76, 714 (2001).

    Article  Google Scholar 

  8. S. DeBeer, D.W. Randall, A.M. Nersissian, J.S. Valentine, B. Hedman, K.O. Hodgson, E.I. Solomon, J. Phys. Chem. B 104, 10814 (2001).

    Article  CAS  Google Scholar 

  9. J. Wong, F.W. Lytle, R.P. Messmer, D.H. Maylotte, Phys. Rev. B 3, 5596 (1984).

    Article  Google Scholar 

  10. D.C. Koningsberger, B.L. Mojet, G.E. van Dorssen, D.E. Ramaker, Top. Catal. 10, 143 (2000).

    Article  CAS  Google Scholar 

  11. M.A. Newton, A.J. Dent, J. Evans, Chem. Soc. Rev. 31, 83 (2002).

    Article  CAS  Google Scholar 

  12. M. Richwin, R. Zaeper, D. Lützenkirchen-Hecht, R. Frahm, J. Synchrotron. Radiat. 8, 354

  13. R. Frahm, M. Richwin, D. Lützenkirchen-Hecht, Physica Scripta T 115, 974 (2005).

    Article  Google Scholar 

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

    Article  CAS  Google Scholar 

  15. A.M. Flank, A. Fontaine, A. Jucha, M. Lemonnier, C. Williams, J. Phys. Lett. 43, L315 (1982).

    Article  Google Scholar 

  16. E. Dooryhee, G.N. Greaves, A.T. Steel, R.P. Townsend, S.W. Carr, J.M. Thomas, C.R.A. Catlow, Faraday Discuss. 89, 119 (1990).

    Article  CAS  Google Scholar 

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

    Article  CAS  Google Scholar 

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

    CAS  Google Scholar 

  19. J. Evans, L. O’Neill, V.L. Kambhampati, G. Rayner, S. Turin, A. Genge, A.J. Dent, T. Neisius, J. Chem. Soc., Dalton Trans., 2207 (2002).

  20. M. Tromp, J.R.A. Sietsma, J.A. van Bokhoven, G.P.F. van Strijdonck, R.J. van Haaren, A.M.J. van der Eerden, P.W.N.M. van Leeuwen, D.C. Koningsberger, Chem. Commun., 128 (2003).

  21. V. Briois, D. Lützenkirchen-Hecht, F. Villain, E. Fonda, S. Belin, B. Griesebock, R. Frahm, J. Phys. Chem. A 109, 320 (2005).

    Article  CAS  Google Scholar 

  22. A.M. Beale, A.M.J. van der Eerden, K. Kervinen, M.A. Newton, B.M. Weckhuysen, Chem. Commun., 3015 (2005).

  23. S.J. Tinnemans, J.G. Mesu, K. Kervinen, T. Visser, T.A. Nijhuis, A.M. Beale, D.E. Keller, A.M.J. van der Eerden, B.M. Weckhuysen, Catal. Today 113, 3 (2006).

    Article  CAS  Google Scholar 

  24. M.K. Oudenhuijzen, P.J. Kooyman, B. Tappel, J.A. van Bokhoven, D.C. Koningsberger, J. Catal. 205, 135 (2002).

    Article  CAS  Google Scholar 

  25. F. Cimini, R. Prins, J. Phys. Chem. B 101, 5277 (1997).

    Article  CAS  Google Scholar 

  26. C. Keresszegi, J.D. Grunwaldt, T. Mallat, A. Baiker, J. Catal. 222, 268 (2004).

    Article  CAS  Google Scholar 

  27. A.E. Russell, A. Rose, Chem. Rev. 104, 3 (2004).

    Article  CAS  Google Scholar 

  28. V.S. Murthi, R.C. Urian, S. Mukerjee, J. Phys. Chem. B 108, 11011 (2004).

    Article  CAS  Google Scholar 

  29. M. Teliska, W.E. O’Grady, D.E. Ramaker, J. Phys. Chem. B 109, 8076 (2005).

    Article  CAS  Google Scholar 

  30. B.S. Clausen, L. Grabaek, G. Steffensen, P.L. Hansen, H. Topsøe, Catal. Lett. 20, 23 (1993).

    Article  CAS  Google Scholar 

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

    Article  CAS  Google Scholar 

  32. J.-D. Grunwaldt, B.S. Clausen, Top. Catal. 18, 37 (2002).

    Article  CAS  Google Scholar 

  33. J.-D. Grunwaldt, M. Caravati, A. Baiker, J. Phys. Chem. B 110, 9916 (2006).

    Article  CAS  Google Scholar 

  34. J.-D. Grunwaldt, S. Hannemann, C.G. Schroer, A. Baiker, J. Phys. Chem. B 110, 8674 (2006).

    Article  CAS  Google Scholar 

  35. N. Yoshida, T. Matsushita, S. Saigo, H. Oyanagi, H. Hashimoto, M. Fujimoto, J. Chem. Soc., Chem. Commun., 354 (1990).

  36. M.B.B.A. Rahman, P.R. Bolton, J. Evans, A.J. Dent, I. Harvey, S. Diaz-Moreno, Faraday Discuss. 122, 211 (2002).

    Article  Google Scholar 

  37. M. Tromp, PhD thesis, Utrecht University, Utrecht, the Netherlands (2004).

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

  39. M.A. Newton, D.G. Burnaby, A.J. Dent, S. Diaz-Moreno, J. Evans, S.G. Fiddy, T. Neisius, S. Pascarelli, S. Turin, J. Phys. Chem. A 105, 5965 (2001).

    Article  CAS  Google Scholar 

  40. M.A. Newton, D.G. Burnaby, A.J. Dent, S. Diaz-Moreno, J. Evans, S.G. Fiddy, T. Neisius, S. Turin, J. Phys. Chem. B 106, 4214 (2002).

    Article  CAS  Google Scholar 

  41. M.A. Newton, A.J. Dent, S. Diaz-Moreno, S.G. Fiddy, J. Evans, Angew. Chem., Int. Ed. 41, 2587 (2002).

    Article  CAS  Google Scholar 

  42. M.A. Newton, A.J. Dent, S. Diaz-Moreno, S.G. Fiddy, B. Jyoti, J. Evans, Chem. Eur. J. 12, 1975 (2006).

    Article  CAS  Google Scholar 

  43. M.A. Newton, B. Jyoti, A.J. Dent, S. Diaz-Moreno, S.G. Fiddy, J. Evans, Chem. Phys. Chem. 5, 1056 (2004).

    Article  CAS  Google Scholar 

  44. N. Sheppard, T.T. Nguyen, Adv. Infrared Raman Spectrosc. 5, 67 (1978).

    CAS  Google Scholar 

  45. M.A. Newton, B. Jyoti, A.J. Dent, S.G. Fiddy, J. Evans, Chem. Commun. 2382 (2004).

  46. A.J. Dent, J. Evans, S.G. Fiddy, B. Jyoti, M.A. Newton, M. Tromp, Angew. Chem., Int. Ed. 46, 5356 (2007).

    Article  CAS  Google Scholar 

  47. K. Hämäläinen, C.C. Kao, J.B. Hastings, D.P. Siddons, L.E. Berman, V. Stojanoff, S.P. Cramer, Phys. Rev. B 46, 14274 (1992).

    Article  Google Scholar 

  48. C.J. Doonan, L. Zhang, C.G. Young, S.J. George, A. Deb, U. Bergman, G.N. George, S.P. Cramer, Inorg. Chem. 44, 2579 (2005).

    Article  CAS  Google Scholar 

  49. K. Hämäläinen, D.P. Siddons, J.B. Hastings, L.E. Berman, Phys. Rev. Lett. 67, 2850 (1991).

    Article  Google Scholar 

  50. F.M.F. de Groot, M.H. Krisch, J. Vogel, Phys. Rev. B 66, 195112 (2002).

    Article  CAS  Google Scholar 

  51. J.A. van Bokhoven, C. Louis, J.T. Miller, M. Tromp, O.V. Safonova, P. Glatzel, Angew. Chem., Int. Ed. 45, 4651 (2006).

    Article  CAS  Google Scholar 

  52. O. Safonova, M. Tromp, J.A. van Bokhoven, F.M.F. de Groot, J. Evans, P. Glatzel, J. Phys. Chem. B 110, 16162 (2006).

    Article  CAS  Google Scholar 

  53. P. Glatzel, U. Bergmann, Coord. Chem. Rev. 249, 65 (2005) and references therein.

    Article  CAS  Google Scholar 

  54. F.M.F. de Groot, Chem. Rev. 101, 1779 (2001) and references therein.

    Article  CAS  Google Scholar 

  55. J. Evans, Phys. Chem. Chem. Phys. 8, 3045 (2006).

    Article  CAS  Google Scholar 

  56. I. Swart, A. Fielicke, B. Redlich, G. Meijer, B.M. Weckhuysen, F.M.F. de Groot, J. Am. Chem. Soc. 129, 2516 (2007).

    Article  CAS  Google Scholar 

  57. W. Gawelda, V.T. Pham, M. Benfatto, Y. Zaushitsyn, M. Kaiser, D. Grolimund, S.L. Johnson, R. Abela, A. Hauser, C. Bressler, M. Chergui, Phys. Rev. Lett. 98, 057401 (2007).

    Article  CAS  Google Scholar 

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Authors
  1. John Evans
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  2. Anna Puig-Molina
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  3. Moniek Tromp
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Evans, J., Puig-Molina, A. & Tromp, M. In Situ EXAFS Characterization of Nanoparticulate Catalysts. MRS Bulletin 32, 1038–1043 (2007). https://doi.org/10.1557/mrs2007.213

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