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Advanced Electron Microscopy Characterization of Nanostructured Heterogeneous Catalysts

  • Jingyue Liu (a1)

Heterogeneous catalysis is one of the oldest nanosciences. Although model catalysts can be designed, synthesized, and, to a certain degree, characterized, industrial heterogeneous catalysts are often chemically and physically complex systems that have been developed through many years of catalytic art, technology, and science. The preparation of commercial catalysts is generally not well controlled and is often based on accumulated experiences. Catalyst characterization is thus critical to developing new catalysts with better activity, selectivity, and/or stability. Advanced electron microscopy, among many characterization techniques, can provide useful information for the fundamental understanding of heterogeneous catalysis and for guiding the development of industrial catalysts. In this article, we discuss the recent developments in applying advanced electron microscopy techniques to characterizing model and industrial heterogeneous catalysts. The importance of understanding the catalyst nanostructure and the challenges and opportunities of advanced electron microscopy in developing nanostructured catalysts are also discussed.

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Ajayan, P.M. & Marks, L.D. (1988). Quasimelting and phases of small particles. Phys Rev Lett60, 585587.

Allpress, J.G. & Sanders, J.V. (1967). Structure and orientation of crystals in deposits of metals on mica. Surf Sci7, 478483.

Barry, J.C., Bursill, L.A., & Sanders, A.V. (1985). Electron microscope images of icosahedral and cuboctahedral (fcc. packing) clusters of atoms. Aust J Phys38, 437448.

Batson, P.E. (1993). Simultaneous STEM imaging and electron-energy-loss spectroscopy with atomic column sensitivity. Nature366, 727728.

Batson, P.E., Dellby, N., & Krivanek, O.L. (2002). Sub-angstrom resolution using aberration corrected electron optics. Nature418, 617620.

Bednarova, L., Lyman, C.E., Rytter, E., & Holmen, A. (2002). Effect of support on the size and composition of highly dispersed Pt-Sn particles. J Catal211, 335346.

Bernal, S., Botana, F.J., Calvino, J.J., Lopez-Cartes, C., Perez-Omil, J.A., & Rodriguez-Izquierdo, J.M. (1998). The interpretation of HREM images of supported metal catalysts using image simulation: Profile view images. Ultramicroscopy72, 135164.

Bernal, S., Calvino, J.J., Cauqui, M.A., Cifredo, G.A., Jobacho, A., & Rodriguez-Izquierdo, J.M. (1993). Metal-support interaction phenomena in rhodium/ceria and rhodium/titania catalysts: Comparative study by high-resolution transmission electron spectroscopy. Appl Catal A: General99, 18.

Bernal, S., Calvino, J.J., Cauqui, M.A., Gatica, J.M., Larese, C., Lopez-Cartes, C., Perez-Omil, J.A., & Pintado, J.M. (1999). Some recent results on metal/support interaction effects in NM/CeO2 (NM: noble metal) catalysts. Catal Today50, 175206.

Boyes, E.D. (1998). High-resolution and low-voltage SEM imaging and chemical microanalysis. Adv Mater10, 12771280.

Browning, N.D., Wallis, D.J., Nellist, P.D., & Pennycook, S.J. (1997). EELS in the STEM: Determination of materials properties on the atomic scale. Micron28, 333348.

Cowley, J.M. (1999). Electron nanodiffraction. Microsc Res Tech46, 7597.

Crew, A.V., Wall, J., & Langmore, J. (1970). Visibility of a single atom. Science168, 13381340.

Darji, R. & Howie, A. (1997). Scattering corrections in small particle imaging. Micron28, 95100.

Datye, A.K. & Smith, D.J. (1992). The study of heterogeneous catalysts by high-resolution electron microscopy. Catal Rev Sci Eng34, 129178.

Gai, P.L. (1998). Direct probing of gas molecule-solid catalyst interactions on the atomic scale. Adv Mater10, 12591263.

Gai, P.L., Goringe, M.J., & Barry, J.C. (1986). HREM image contrast from supported small metal particles. J Microsc142, 924.

GaiBoyes, P.L. (1992). Defects in oxide catalysts-fundamental-studies of catalysis in action. Catal Rev Sci Eng34, 154.

Garzon, I.L., Michaelian, K., Beltran, M.R., Posada-Amarillas, A., Ordejon, P., Artacho, E., Sanches-Portal, D., & Soler, J.M. (1998). Lowest energy structures of gold nanoclusters. Phys Rev Lett81, 16001603.

Hansen, T.W., Wagner, J.B., Hansen, P.L., Dahl, S., Topsoe, H., & Jacobsen, C.J.H. (2001). Atomic-resolution in situ transmission electron microscopy of a promoter of a heterogeneous catalyst. Science294, 15081510.

Hansen, P.L., Wagner, J.B., Helveg, S., Rostrup-Nielsen, J.R., Clausen, B.S., & Topsoe, H. (2002). Atom-resolved imaging of dynamic shape changes in supported copper nanocrystals. Science295, 20532055.

Haruta, M. (1997). Size- and support-dependency in the catalysis of gold. Catal Today36, 153166.

Heinemann, K. & Soria, F. (1986). On the detection and size classification of nanometer-size metal particles on amorphous substrates. Ultramicroscopy20, 114.

Ino, S. (1966). Epitaxial growth of metals on rock salt faces cleaved in vacuum. II. Orientation and structure of gold particles formed in ultra-high vacuum. J Phys Soc Jpn21, 346362.

Jose-Yacaman, M. & Avalos-Borja, M. (1992). Electron microscopy of metallic nano particles using high- and medium-resolution techniques. Catal Rev Sci Eng34, 55127.

Jose-Yacaman, M., Marin-Almazo, M., & Ascencio, J.A. (2001). High resolution TEM studies on palladium nanoparticles. J Mol Catal A: Chemical173, 6174.

Joy, D.C. & Joy, C.S. (1996). Low voltage scanning electron microscopy. Micron27, 247263.

Joy, D.C. & Pawley, J.B. (1992). High-resolution scanning electron microscopy. Ultramicroscopy47, 80100.

Klie, R.F., Disko, M.M., & Browning, N.D. (2002). Atomic scale observations of the chemistry at the metal-oxide interface in heterogeneous catalysts. J Catal205, 16.

Liu, J. (2000b). High-resolution and low-voltage FE-SEM imaging and microanalysis in materials characterization. Mater Charact44, 353363.

Liu, J. & Cowley, J.M. (1987). High-resolution scanning electron microscopy of surface reactions. Ultramicroscopy23, 463472.

Liu, J. & Cowley, J.M. (1990). High-angle ADF and high-resolution SE imaging of supported catalyst clusters. Ultramicroscopy34, 119128.

Logan, A.D., Braunschweig, E., Datye, A.K., & Smith, D.J. (1988). Direct observation of the surfaces of small metal crystallites: Rhodium supported on titania. Lanngmuir4, 827830.

Logan, A.D., Braunschweig, E., Datye, A.K., & Smith, D.J. (1989). The oxidation of small rhodium metal particles. Ultramicroscopy31, 132137.

Lyman, C.E. (1986). Digital X-ray imaging of small particles. Ultramicroscopy20, 11924.

Lyman, C.E., Goldstein, J.I., Williams, D.B., Ackland, D.W., Von Harrach, S., Nicholls, A.W., & Statham, P.J. (1994). High-performance X-ray-detection in a new analytical electron-microscope. J Microsc176, 8598.

Lyman, C.E., Lakis, R.E., & Stenger, H.G. Jr. (1995). X-ray emission spectrometry of phase separation in Pt-Rh nanoparticles for nitric oxide reduction. Ultramicroscopy58, 2534.

Malm, J.O. & O'Keefe, M.A. (1997). Deceptive “lattice spacings” in high-resolution micrographs of metal nanoparticles. Ultramicroscopy68, 1323.

Marks, L.D. (1994). Experimental studies of small particle structures. Rep Prog Phys57, 603649.

Marks, L.D. & Smith, D.J. (1981). High-resolution studies of small particles of gold and silver. I. Multiply-twinned particles. J Cryst Growth54, 425432.

Midgley, P.A., Weyland, M., Thomas, J.M., Gai, P.L., & Boyes, E.D. (2002). Probing the spatial distribution and morphology of supported nanoparticles using Rutherford-scattered electron imaging. Angew Chem Int Ed41, 38043807.

Muller, D.A. & Mills, M.J. (1999). Electron microscopy: Probing the atomic structure and chemistry of grain boundaries, interfaces, and defects. Mater Sci Eng A260, 1228.

Nellist, P.D. & Pennycook, S.J. (1996). Direct imaging of the atomic configuration of ultradispersed catalysts. Science274, 413415.

Oleshko, V.P., Crozier, P.A., Cantrell, R.D., & Westwood, A.D. (2001). In situ real-time environmental TEM of gas phase Ziegler-Natta catalytic polymerization of propylene. J Electron Microsc51, S27S39.

Silcox, J. (1998). Core-loss EELS. Curr Opin Solid State Mater Sci3, 336342.

Smith, D.J. (1997). The realization of atomic resolution with the electron microscope. Rep Prog Phys60, 15131580.

Smith, D.J., Yao, M.H., Allard, L.F., & Datye, A.K. (1995). High-resolution scanning electron microscopy for the characterization of supported catalysts. Catal Lett31, 5764.

Strongin, D.R., Bare, S.R., & Somorjai, G.A. (1987a). The importance of C7 sites and surface roughness in the ammonia synthesis reaction over iron. J Catal103, 213215.

Strongin, D.R., Bare, S.R., & Somorjai, G.A. (1987b). The effects of aluminum oxide in restructuring iron single crystal surfaces for ammonia synthesis. J Catal103, 289301.

Sun, K., Liu, J., & Browning, N.D. (2002a). Correlated atomic resolution microscopy and spectroscopy studies of Sn(Sb)O2 nanophase catalysts. J Catal205, 266277.

Sun, K., Liu, J., Nag, N.K., & Browning, N.D. (2002b). Studying the metal-support interaction in Pd/γ-Al2O3 catalysts by atomic-resolution electron energy-loss spectroscopy. Catal Lett84, 193199.

Sun, K., Liu, J., Nag, N.K., & Browning, N.D. (2002c). Atomic scale characterization of supported Pd-Cu/γ-Al2O3 bimetallic catalysts. J Phys Chem B106, 1223912246.

Tanaka, N., Kimita, H., & Kizuka, T. (1996). Time-resolved high-resolution electron microscopy of surface-diffusion of tungsten atoms on MgO(001) surfaces. J Electron Microsc45, 113118.

Tehuacanero, S., Herrera, R., Avalos, M., & Jose-Yacaman, M. (1992). High resolution TEM studies of gold and palladium nano-particles. Acta Metall Mater40, 16631674.

Thomas, J.M., Terasaki, O., Gai, P.L., Zhou, W.Z., & Gonzalez-Calbet, J. (2001). Structural elucidation of microporous and mesoporous catalysts and molecular sieves by high-resolution electron microscopy. Acc Chem Res34, 583594.

Treacy, M.M.J. & Rice, S.B. (1989). Catalyst particle sizes from Rutherford scattered intensities. J Microscopy156, 211234.

Tsen, S.C.Y., Crozier, P.A., & Liu, J. (2003). Lattice measurement and alloy compositions in metal and bimetallic nanoparticles. Ultramicroscopy98, 6372.

Yao, M.H. & Smith, D.J. (1994). HREM image simulations for small-particle catalysts on crystalline supports. J Microsc175, 252265.

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Microscopy and Microanalysis
  • ISSN: 1431-9276
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