Skip to main content Accessibility help

In Situ EXAFS Characterization of Nanoparticulate Catalysts

  • John Evans, Anna Puig-Molina and Moniek Tromp


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.



Hide All
1.D.C., Koningsberger, R., Prins, Eds., X-ray Absorption, Principles, Applications, Techniques of EXAFS, SEXAFS and XANES (Wiley Interscience, New York, 1988).
2.Brinkgreve, P., Koningsberger, D.C., Patent Application NL8300927 (1983).
3.Ravet, M.F., Krill, G., Rev. Sci. Instrum. 54, 227 (1983).
4.Williams, A., Rev. Sci. Instrum. 54, 193 (1983).
5.Yamashita, S., Taniguchi, K., Nomoto, S., Yamaguchi, T., Wakita, H., X-ray Spectrom. 21, 91 (1992).
6.Tromp, M., van Bokhoven, J.A., van Strijdonck, G.P.F., van Leeuwen, P.W.N.M., Koningsberger, D.C., Ramaker, D.E., J. Am. Chem. Soc. 127, 777 (2005).
7.Wilke, M., Farges, F., Petit, P.E., Brown, G.E., Martin, F., Am. Mineral. 76, 714 (2001).
8.DeBeer, S., Randall, D.W., Nersissian, A.M., Valentine, J.S., Hedman, B., Hodgson, K.O., Solomon, E.I., J. Phys. Chem. B 104, 10814 (2001).
9.Wong, J., Lytle, F.W., Messmer, R.P., Maylotte, D.H., Phys. Rev. B 3, 5596 (1984).
10.Koningsberger, D.C., Mojet, B.L., van Dorssen, G.E., Ramaker, D.E., Top. Catal. 10, 143 (2000).
11.Newton, M.A., Dent, A.J., Evans, J., Chem. Soc. Rev. 31, 83 (2002).
12.Richwin, M., Zaeper, R., Lützenkirchen-Hecht, D., Frahm, R., J. Synchrotron. Radiat. 8, 354 (2001).
13.Frahm, R., Richwin, M., Lützenkirchen-Hecht, D., Physica Scripta T 115, 974 (2005).
14.Matsushita, T., Phizackerley, R.P., Jpn. J. Appl. Phys. 20, 2223 (1981).
15.Flank, A.M., Fontaine, A., Jucha, A., Lemonnier, M., Williams, C., J. Phys. Lett. 43, L315 (1982).
16.Dooryhee, E., Greaves, G.N., Steel, A.T., Townsend, R.P., Carr, S.W., Thomas, J.M., Catlow, C.R.A., Faraday Discuss. 89, 119 (1990).
17.Couves, J.W., Thomas, J.M., Waller, D., Jones, R.H., Dent, A.J., Derbyshire, G.E., Greaves, G.N., Nature 354, 465 (1991).
18.Clausen, B.S., Topsøe, H., Frahm, R., Adv. Catal. 42, 315 (1998).
19.Evans, J., O'Neill, L., Kambhampati, V.L., Rayner, G., Turin, S., Genge, A., Dent, A.J., Neisius, T., J. Chem. Soc., Dalton Trans., 2207 (2002).
20.Tromp, M., Sietsma, J.R.A., van Bokhoven, J.A., van Strijdonck, G.P.F., van Haaren, R.J., van der Eerden, A.M.J., van Leeuwen, P.W.N.M., Koningsberger, D.C., Chem. Commun., 128 (2003).
21.Briois, V., Lützenkirchen-Hecht, D., Villain, F., Fonda, E., Belin, S., Griesebock, B., Frahm, R., J. Phys. Chem. A 109, 320 (2005).
22.Beale, A.M., van der Eerden, A.M.J., Kervinen, K., Newton, M.A., Weckhuysen, B.M., Chem. Commun., 3015 (2005).
23.Tinnemans, S.J., Mesu, J.G., Kervinen, K., Visser, T., Nijhuis, T.A., Beale, A.M., Keller, D.E., van der Eerden, A.M.J., Weckhuysen, B.M., Catal. Today 113, 3 (2006).
24.Oudenhuijzen, M.K., Kooyman, P.J., Tappel, B., van Bokhoven, J.A., Koningsberger, D.C., J. Catal. 205, 135 (2002).
25.Cimini, F., Prins, R., J. Phys. Chem. B 101, 5277 (1997).
26.Keresszegi, C., Grunwaldt, J.D., Mallat, T., Baiker, A., J. Catal. 222, 268 (2004).
27.Russell, A.E., Rose, A., Chem. Rev. 104, 3 (2004).
28.Murthi, V.S., Urian, R.C., Mukerjee, S., J. Phys. Chem. B 108, 11011 (2004).
29.Teliska, M., O'Grady, W.E., Ramaker, D.E., J. Phys. Chem. B 109, 8076 (2005).
30.Clausen, B.S., Grabaek, L., Steffensen, G., Hansen, P.L., Topsøe, H., Catal. Lett. 20, 23 (1993).
31.Grunwaldt, J.-D., Molenbroek, A.M., Topsøe, N.-Y., Topsøe, H., Clausen, B.S., J. Catal. 194, 452 (2000).
32.Grunwaldt, J.-D., Clausen, B.S., Top. Catal. 18, 37 (2002).
33.Grunwaldt, J.-D., Caravati, M., Baiker, A., J. Phys. Chem. B 110, 9916 (2006).
34.Grunwaldt, J.-D., Hannemann, S., Schroer, C.G., Baiker, A., J. Phys. Chem. B 110, 8674 (2006).
35.Yoshida, N., Matsushita, T., Saigo, S., Oyanagi, H., Hashimoto, H., Fujimoto, M., J. Chem. Soc., Chem. Commun., 354 (1990).
36. M.Rahman, B.B.A., Bolton, P.R., Evans, J., Dent, A.J., Harvey, I., Diaz-Moreno, S., Faraday Discuss. 122, 211 (2002).
37.Tromp, M., PhD thesis, Utrecht University, Utrecht, the Netherlands (2004).
38.Fiddy, S.G., Newton, M.A., Dent, A.J., Salvini, G., Corker, J.M., Turin, S., Campbell, T., Evans, J., Chem. Commun., 851 (1999).
39.Newton, M.A., Burnaby, D.G., Dent, A.J., Diaz-Moreno, S., Evans, J., Fiddy, S.G., Neisius, T., Pascarelli, S., Turin, S., J. Phys. Chem. A 105, 5965 (2001).
40.Newton, M.A., Burnaby, D.G., Dent, A.J., Diaz-Moreno, S., Evans, J., Fiddy, S.G., Neisius, T., Turin, S., J. Phys. Chem. B 106, 4214 (2002).
41.Newton, M.A., Dent, A.J., Diaz-Moreno, S., Fiddy, S.G., Evans, J., Angew. Chem., Int. Ed. 41, 2587 (2002).
42.Newton, M.A., Dent, A.J., Diaz-Moreno, S., Fiddy, S.G., Jyoti, B., Evans, J., Chem. Eur. J. 12, 1975 (2006).
43.Newton, M.A., Jyoti, B., Dent, A.J., Diaz-Moreno, S., Fiddy, S.G., Evans, J., Chem. Phys. Chem. 5, 1056 (2004).
44.Sheppard, N., Nguyen, T.T., Adv. Infrared Raman Spectrosc. 5, 67 (1978).
45.Newton, M.A., Jyoti, B., Dent, A.J., Fiddy, S.G., Evans, J., Chem. Commun. 2382 (2004).
46.Dent, A.J., Evans, J., Fiddy, S.G., Jyoti, B., Newton, M.A., Tromp, M., Angew. Chem., Int. Ed. 46, 5356 (2007).
47.Hämäläinen, K., Kao, C.C., Hastings, J.B., Siddons, D.P., Berman, L.E., Stojanoff, V., Cramer, S.P., Phys. Rev. B 46, 14274 (1992).
48.Doonan, C.J., Zhang, L., Young, C.G., George, S.J., Deb, A., Bergman, U., George, G.N., Cramer, S.P., Inorg. Chem. 44, 2579 (2005).
49.Hämäläinen, K., Siddons, D.P., Hastings, J.B., Berman, L.E., Phys. Rev. Lett. 67, 2850 (1991). Groot, F.M.F., Krisch, M.H., Vogel, J., Phys. Rev. B 66, 195112 (2002).
51.van Bokhoven, J.A., Louis, C., Miller, J.T., Tromp, M., Safonova, O.V., Glatzel, P., Angew. Chem., Int. Ed. 45, 4651 (2006).
52.Safonova, O., Tromp, M., van Bokhoven, J.A., de Groot, F.M.F., Evans, J., Glatzel, P., J. Phys. Chem. B 110, 16162 (2006).
53.Glatzel, P., Bergmann, U., Coord. Chem. Rev. 249, 65 (2005) and references therein. Groot, F.M.F., Chem. Rev. 101, 1779 (2001) and references therein.
55.Evans, J., Phys. Chem. Chem. Phys. 8, 3045 (2006).
56.Swart, I., Fielicke, A., Redlich, B., Meijer, G., Weckhuysen, B.M., de Groot, F.M.F., J. Am. Chem. Soc. 129, 2516 (2007).
57.Gawelda, W., Pham, V.T., Benfatto, M., Zaushitsyn, Y., Kaiser, M., Grolimund, D., Johnson, S.L., Abela, R., Hauser, A., Bressler, C., Chergui, M., Phys. Rev. Lett. 98, 057401 (2007).

In Situ EXAFS Characterization of Nanoparticulate Catalysts

  • John Evans, Anna Puig-Molina and Moniek Tromp


Full text views

Total number of HTML views: 0
Total number of PDF views: 0 *
Loading metrics...

Abstract views

Total abstract views: 0 *
Loading metrics...

* Views captured on Cambridge Core between <date>. This data will be updated every 24 hours.

Usage data cannot currently be displayed