Advanced Electron Microscopy Characterization of Nanostructured Heterogeneous Catalysts

Microscopy and Microanalysis

Volumn 10, Issue 1, 2004, Pages 55-76

  Liu, Jingyue ^a  

^a MONSANTO COMPANY   (United States)

Author keywords

Catalyst characterization; EDS; EELS; Electron microscopy; Heterogeneous catalyst; HREM; Nanoparticles; Nanostructure; SEM; STEM; Surface

Indexed keywords

COPPER; HEAVY METAL; PALLADIUM;

CATALYSIS; CONFERENCE PAPER; ELECTRON MICROSCOPY; INSTRUMENTATION; METHODOLOGY; NANOTECHNOLOGY; PARTICLE SIZE;

CATALYSIS; COPPER; METALS, HEAVY; MICROSCOPY, ELECTRON; NANOTECHNOLOGY; PALLADIUM; PARTICLE SIZE;

EID: 1442338810     PISSN: 14319276     EISSN: None     Source Type: Journal    
DOI: 10.1017/S1431927604040310     Document Type: Conference Paper

References (72)

1. AJAYAN, P.M. & MARKS, L.D. (1988). Quasimelting and phases of small particles. Phys Rev Lett 60, 585-587.
2. ALLPRESS, J.G. & SANDERS, J.V. (1967). Structure and orientation of crystals in deposits of metals on mica. Surf Sci 7, 478-483.
3. BARRY, J.C., BURSILL, L.A. & SANDERS, A.V. (1985). Electron microscope images of icosahedral and cuboctahedral (fcc. packing) clusters of atoms. Aust J Phys 38, 437-448.
4. BATSON, P.E. (1993). Simultaneous STEM imaging and electron-energy-loss spectroscopy with atomic column sensitivity. Nature 366, 727-728.
5. BATSON, P.E., DELLBY, N. & KRIVANEK, O.L. (2002). Sub-angstrom resolution using aberration corrected electron optics. Nature 418, 617-620.
6. 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 Catal 211, 335-346.
7. 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. Ultramicroscopy 72, 135-164.
8. 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: General 99, 1-8.
9. 2 (NM: noble metal) catalysts. Catal Today 50, 175-206.
10. BOYES, E.D. (1998). High-resolution and low-voltage SEM imaging and chemical microanalysis. Adv Mater 10, 1277-1280.
11. BROWNING, N.D., ARSLAN, I., ITO, Y., JAMES, E. M., KLIE, R.F., MOECK, P., TOPURIA, T. & XIN, Y. (2001). Application of atomic scale STEM techniques to the study of interfaces and defects in materials. J Electron Microsc 50, 205-218.
12. 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. Micron 28, 333-348.
13. COWLEY, J.M. (1999). Electron nanodiffraction. Microsc Res Tech 46, 75-97.
14. CREW, A.V., WALL, J. & LANGMORE, J. (1970). Visibility of a single atom. Science 168, 1338-1340.
15. CROZIER, P.A., TSEN, S.-C.Y., LOPES-CARTES, C., LIU, J. & CALVINO, J.J. (1999). Factors affecting the accuracy of lattice spacing determination by HREM in nanometre-sized Pt particles. J Electron Microsc 48, 1015-1024.
16. DARJI, R. & HOWIE, A. (1997). Scattering corrections in small particle imaging. Micron 28, 95-100.
17. DATYE, A.K. & SMITH, D.J. (1992). The study of heterogeneous catalysts by high-resolution electron microscopy. Catal Rev Sci Eng 34, 129-178.
18. ERTL, G. (2002). Heterogeneous catalysis on atomic scale. J Mol Catal A: Chemical 3443, 1-12.
19. GAI, RL. (1998). Direct probing of gas molecule-solid catalyst interactions on the atomic scale. Adv Mater 10, 1259-1263.
20. GAI, RL. (2002). Developments in in situ environmental cell high-resolution electron microscopy and applications to catalysis. Top Catal 21, 161-173.
21. GAI, P.L., GORINGE, M.J. & BARRY, J.C. (1986). HREM image contrast from supported small metal particles. J Microsc 142, 9-24.
22. GAI, P.L., KOURTAKIS, K. & ZIEMECKI, S. (2000). In situ real-time environmental high resolution electron microscopy of nanometer size novel xerogel catalysts for hydrogenation reactions in nylon 6,6. Microsc Microanal 6, 335-342.
23. GAIBOYES, RL. (1992). Defects in oxide catalysts-fundamental-studies of catalysis in action. Catal Rev Sci Eng 34, 1-54.
24. GARZON, I.L., MICHAELIAN, K., BELTRAN, M.R., POSADA-AMARILLAS, A., ORDEJON, R, ARTACHO, E., SANCHES-PORTAL, D. & SOLER, J.M. (1998). Lowest energy structures of gold nanoclusters. Phys Rev Lett 81, 1600-1603.
25. 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. Science 294, 1508-1510.
26. 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. Science 295, 2053-2055.
27. HARUTA, M. (1997). Size-and support-dependency in the catalysis of gold. Catal Today 36, 153-166.
28. HEINEMANN, K. & SORIA, F. (1986). On the detection and size classification of nanometer-size metal particles on amorphous substrates. Ultramicroscopy 20, 1-14.
29. 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 Jpn 21, 346-362.
30. JOSE-YACAMAN, M. & AVALOS-BORJA, M. (1992). Electron microscopy of metallic nano particles using high-and medium-resolution techniques. Catal Rev Sci Eng 34, 55-127.
31. JOSE-YACAMANN, M., DIAZ, G. & GOMEZ, A. (1995). Electron microscopy of catalysts; the present, the future and the hopes. Catal Today 32, 161-199.
32. JOSE-YACAMAN, M., MARIN-ALMAZO, M. & ASCENCIO, J.A. (2001). High resolution TEM studies on palladium nanoparticles. J Mol Catal A: Chemical 173, 61-74.
33. JOY, D.C. & JOY, C.S. (1996). Low voltage scanning electron microscopy. Micron 27, 247-263.
34. JOY, D.C. & PAWLEY, J.B. (1992). High-resolution scanning electron microscopy. Ultramicroscopy 47, 80-100.
35. 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 Catal 205, 1-6.
36. LIU, J. (1998). Low voltage high-resolution secondary electron microscopy of industrial supported catalysts. In Proceedings of the 14th ICEM: Electron Microscopy, Benavides, H.A.C. & Yacaman, M.J. (Eds). Vol. 2, pp. 399-400. Bristol: Institute of Physics Publishing.
37. LIU, J. (2000a). Contrast of highly dispersed metal nanoparticles in high-resolution secondary electron and backscattered electron images of supported metal catalysts. Microsc Microanal 6, 388-399.
38. LIU, J. (2000b). High-resolution and low-voltage FE-SEM imaging and microanalysis in materials characterization. Mater Charact 44, 353-363.
39. LIU, J. (2002). HAADF imaging of metal nanoclusters and nanoparticles: Challenges and opportunities. In Proceedings of the 15th International Congress on Electron Microscopy, pp. 499-500.
40. LIU, J. & COWLEY, J.M. (1987). High-resolution scanning electron microscopy of surface reactions. Ultramicroscopy 23, 463-472.
41. LIU, J. & COWLEY, J.M. (1990). High-angle ADF and high-resolution SE imaging of supported catalyst clusters. Ultramicroscopy 34, 119-128.
42. 2. In Proceedings of the 18th North American Catalysis Society Meeting, p. 225.
43. LIU, J., ORNBERG, R.L. & EBNER, J.R. (1997). Studies of supported metal catalysts using low voltage biased secondary electron imaging in a JSM-6320F FE-SEM. Microsc Microanal 3 (Suppl. 2), 1123-1224.
44. LIU, J. & SPINNLER, G.E. (1994). Observation of the evolution of 55-atom icosahedral Ag clusters by coherent electron nanodiffraction in a UHV STEM. In Proceedings of the Microscopy Society of America, Bailey, G.W. & Garratt-Reed, A.J. (Eds.), pp. 788-789. San Francisco: San Francisco Press, Inc.
45. 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. Lanngmuir 4, 827-830.
46. LOGAN, A.D., BRAUNSCHWEIG, E., DATYE, A.K. & SMITH, D.J. (1989). The oxidation of small rhodium metal particles. Ultramicroscopy 31, 132-137.
47. LYMAN, C.E. (1986). Digital X-ray imaging of small particles. Ultramicroscopy 20, 119-24.
48. 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 Microsc 176, 85-98.
49. 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. Ultramicroscopy 58, 25-34.
50. LYMAN, C.E., LAKIS, ROLLIN E., STENGER, H.G., JR., TOTDAL, B. & PRESTVIK, R. (2000). Analysis of alloy nanoparticles. Mikrochim Acta 132, 301-308.
51. MALM, J.O. & O'KEEFE, M.A. (1997). Deceptive "lattice spacings" in high-resolution micrographs of metal nanoparticles. Ultramicroscopy 68, 13-23.
52. MARKS, L.D. (1994). Experimental studies of small particle structures. Rep Prog Phys 57, 603-649.
53. MARKS, L.D. & SMITH, D.J. (1981). High-resolution studies of small particles of gold and silver. I. Multiply-twinned particles. J Cryst Growth 54, 425-432.
54. MIDGLEY, P.A., WEYLAND, M., THOMAS, J.M., GAI, RL. & BOYES, E.D. (2002). Probing the spatial distribution and morphology of supported nanoparticles using Rutherford-scattered electron imaging. Angew Chem Int Ed 41, 3804-3807.
55. MULLER, D.A. & MILLS, M.J. (1999). Electron microscopy: Probing the atomic structure and chemistry of grain boundaries, interfaces, and defects. Mater Sci Eng A 260, 12-28.
56. NELLIST, P.D. & PENNYCOOK, S.J. (1996). Direct imaging of the atomic configuration of ultradispersed catalysts. Science 274, 413-415.
57. 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 Microsc 51, S27-S39.
58. SILCOX, J. (1998). Core-loss EELS. Curr Opin Solid State Mater Sci 3, 336-342.
59. SMITH, D.J. (1997). The realization of atomic resolution with the electron microscope. Rep Prog Phys 60, 1513-1580.
60. 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 Lett 31, 57-64.
61. 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 Catal 103, 213-215.
62. 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 Catal 103, 289-301.
63. SUN, K., LIU, J. & BROWNING, N.D. (2002a). Correlated atomic resolution microscopy and spectroscopy studies of Sn(Sb)O2 nanophase catalysts. J Catal 205, 266-277.
64. 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 Lett 84, 193-199.
65. 3 bimetallic catalysts. J Phys Chem B 106, 12239-12246.
66. 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 Microsc 45, 113-118.
67. TEHUACANERO, S., HERRERA, R., AVALOS, M. & JOSE-YACAMAN, M. (1992). High resolution TEM studies of gold and palladium nano-particles. Acta Metall Mater 40, 1663-1674.
68. 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 Res 34, 583-594.
69. TREACY, M.M.J. & RICE, S.B. (1989). Catalyst particle sizes from Rutherford scattered intensities. J Microscopy 156, 211-234.
70. TSEN, S.C.Y., CROZIER, P.A. & LIU, J. (2003). Lattice measurement and alloy compositions in metal and bimetallic nanoparticles. Ultramicroscopy 98, 63-72.
71. WILLIAMS, D.B. & CARTER, C.B. (1996). Transmission Electron Microscopy. New York: Plenum Press.
72. YAO, M.H. & SMITH, D.J. (1994). HREM image simulations for small-particle catalysts on crystalline supports. J Microsc 175, 252-265.