Abstract
Heterogeneous catalysts are an important set of materials that increase the rate of chemical reactions. The increase in the reaction rate can be many orders of magnitude and depends on the degree to which the activation energy of the reaction can be lowered. Heterogeneous catalysts have traditionally played major roles in fields such as fuel processing, chemical synthesis and polymer production (van Santen et al. 1999). More recently they have played increasing roles in the environmental technology, energy production and materials synthesis. The field is undergoing a significant expansion and it is widely recognized that, for substantial progress, it is necessary to develop an atomic-level understanding of the interaction between the catalyst and the reactants/product in order to design novel catalytic materials that can address the problems of the 21 st century.
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References
L.F. Allard, W.C. Bigelow, D.P. Nackashi, J. Damiano, S.E. Mick, A new paradigm for ultra-high-resolution imaging at elevated temperature. Microsc. Microanal. 14(Suppl. 2), 792–793 (2008)
L.F. Allard, W.C. Bigelow, M. Jose-Yacaman, D.P. Nackashi, J. Damiano, S.E. Mick, A new MEMS-based system for ultra-high-resolution imaging at elevated temperatures. Microsc. Res. Tech. 72, 208–215 (2009)
I. Arslan, J.C. Walmsley, E. Rytter, E. Bergene, P.A. Midgley, Toward three-dimensional nanoengineering of heterogeneous catalysts. J. Am. Chem. Soc. 130, 5716–5719 (2008)
R.T.K. Baker, M.A. Barber, P.S. Harris, F.S. Feates, R.J. White, Nucleation and growth of carbon deposits from the nickel catalyzed decomposition of acetylene. J. Catal. 26, 51–62 (1972)
R.T.K. Baker, J.J. Chludzinski, Filamentous carbon growth on nickel-iron surfaces: The effect of various oxide additives. J. Catal. 64, 464–478 (1980)
R.T.K. Baker, J.J. Chludzinski, In-situ electron microscopy studies of the behavior of supported ruthenium particles. 1. The catalytic influence on graphite gasification reactions. J. Phys. Chem. 90, 4730–4734 (1986)
R.T.K. Baker, J.J. Chludzinski, J.A. Dumesic, Filamentous carbon growth on nickel surfaces treated with titanium dioxide: Migration of titania and ramifications of strong metal–support interactions. J. Catal. 93, 312–320 (1985)
R.T.K. Baker, J.J. Chludzinski, C.R.F. Lund, Further studies of the formation of filamentous carbon from the interaction of supported iron particles with acetylene. Carbon 25, 295–303 (1987)
R.T.K. Baker, P.S. Harris, R.B. Thomas, R.J. Waite, Formation of filamentous carbon from iron, cobalt and chromium catalyzed decomposition of acetylene. J. Catal. 30, 86–95 (1973)
R.T.K. Baker, N.M. Rodriguez, A review of the use of in situ electron microscopy techniques for the study of iron-based catalysts for coal conversion processes. Energy Fuels 8, 330–340 (1994)
M.A. Bañares, I.E. Wachs, Molecular structures of supported metal oxide catalysts under different environments. J. Raman Spectrosc. 33, 359 (2002)
P.E. Batson, Motion of Au atoms on carbon in the aberration corrected STEM. Microsc. Microanal. 14, 89–97 (2008)
L. Bednarova, C.E. Lyman, E. Rytter, A. Holmen, Effect of support on the size and composition of highly dispersed Pt–Sn particles. J. Catal. 211, 335–346 (2002)
A.R. Belambe, R. Oukaci, J.G.J. Goodwin, Effect of pretreatment on the activity of a Ru-promoted Co/Al2O3 Fischer Tropsch catalyst. J. Catal. 166, 8–15 (1997)
D.A. Blom, L.F. Allard, S. Mishina, O’M.A. Keefe, Early results from an aberration-corrected JEOL 2200FS STEM/TEM at Oak Ridge National Laboratory. Microsc. Microanal. 12, 483–491 (2006)
D.A. Blom, S.A. Bradley, W. Sinkler, L.F. Allard, Observation of Pt atoms, clusters and rafts on oxide supports, by sub-Angstrom Z-contrast imaging in an aberration-corrected STEM/TEM. Microsc. Microanal. 12(Suppl. 2), 50–51 (2006)
A.Y. Borisevich, A.R. Lupini, S.J. Pennycook, Depth sectioning with the aberration-corrected scanning transmission electron microscope. Proc. Natl. Acad. Sci. 103, 3044–3048 (2006)
A.Y. Borisevich, S. Wang, S.N. Rashkeev, M. Glazoff, S.J. Pennycook, S.T. Pantelides, Dual nanoparticle/substrate control of catalytic dehydrogenation. Adv. Mater. 19, 2129–2133 (2007)
E.D. Boyes, P.L. Gai, Environmental high resolution electron microscopy and applications to chemical science. Ultramicroscopy 67, 219–232 (1997)
P. Butler, K. Hale, Dynamic experiments in the electron microscope. Prac. Methods Electron Microsc., North Holland 9, 239–308 (1981)
J.F. Creemer, S. Helveg, et al., Atomic-scale electron microscopy at ambient pressure. Ultramicroscopy 108, 993–998 (2008)
A.V. Crewe, J. Wall, J. Langmore, Visibility of single atoms. Science 168, 1338–1340 (1970)
P.A. Crozier, Nanoscale oxide patterning with electron–solid–gas reactions. Nanoletters 7, 2395–2398 (2007)
P.A. Crozier, A.K. Datye, Direct observation of reduction of PdO to Pd metal by in situ electron microscopy. Stud. Surf. Sci. Catal. 130, 3119–3124 (2000)
P.A. Crozier, R. Sharma, A.K. Datye, Oxidation and reduction of small palladium particles on silica. Microsc. Microanal. 4, 278–285 (1998)
P.A. Crozier, S.-C. Tsen, J. Liu, C. Lopez Cartes, J.A. Perez-Omil, Factors affecting the accuracy of lattice spacing determination by HREM in nanometre-sized Pt particles. J. Electron Microsc. 48(Suppl.), 1015–1024 (1999)
P.A. Crozier, R. Wang, R. Sharma, In situ environmental TEM studies of dynamic changes in cerium-based oxide nanoparticles during redox processes. Ultramicroscopy 108, 1432–1440 (2008)
A.K. Datye, Electron microscopy of catalysts: recent achievements and future prospects. J. Catal. 216, 144–154 (2003)
A.K. Datye, Particle size distributions in heterogeneous catalysts: What do they tell us about the sintering mechanism? Catal. Today 111, 59–67 (2006)
N. de Jonge, D.B. Peckys, G.J. Kremers, D.W. Piston, Electron microscopy of whole cells in liquid with nanometer resolution. Proc. Natl. Acad. Sci. USA. 106, 2159–2164 (2009)
N. Dellby, M. Murfitt, O.L. Krivanek, M. Kociak, K. March, M. Tence, C. Colliex, Atomic-resolution STEM at 60 kV primary voltage. Microsc. Microanal. 14(Suppl 2), 136–137 (2008)
E.G. Derouane, J.J. Chludzinski, R.T.K. Baker, Direct observation of wetting and spreading of copper particles on magnesium oxide. J. Catal. 85, 187–196 (1984)
A.M. Donald, A.J. Craven, A study of grain boundary segregation in Cu–Bi alloys using STEM. Philos. Mag. A 39, 1–11 (1979)
R.C. Doole, G.M. Parkinson, J.M. Stead, Inst. Phys. Conf. Ser. 119, 157–160 (1991)
J.A. Dumesic, S.A. Stevenson, R.D. Sherwood, R.T.K. Baker, Migration of nickel and titanium oxide species as studied by in situ scanning transmission electron microscopy. J. Catal. 99, 79–87 (1986)
R.F. Egerton, Electron Energy-Loss Spectroscopy in the Electron Microscope, 2nd edn. (Plenum Press, New York, NY, 1996)
R.F. Egerton, Application of electron energy-loss spectroscopy to the study of solid catalysts. Top. Catal. 21, 185–190 (2002)
R.F. Egerton, Electron energy-loss spectroscopy in the TEM. Rep. Prog. Phys. 72, 016502 (2009)
D. Ferrer, D.A. Blom, L.F. Allard, S. Mejia, E. Perez-Tijerina, M. Jose-Yacaman, Atomic structure of three-layer Au/Pd nanoparticles revealed by aberration-corrected scanning transmission electron microscopy. J. Mater. Chem. 18, 2442–2446 (2008)
P.L. Gai, Philos. Mag. 48, 359–371 (1983)
P.L. Gai, Environmental high resolution electron microscopy of gas-catalyst reactions. Top. Catal. 8, 97–113 (1999)
P.L. Gai, E.D. Boyes, Catal. Rev. Sci. Eng. 34, 1–54 (1992)
P.L. Gai, E.D. Boyes, in In Situ Microscopy in Materials Research, ed. by P.L. Gai (Kluwer, Dordrecht, 1997), pp. 123–146
S. Giorgio, S. Sao Joao, S. Nitsche, D. Chaudanson, G. Sitja, H.C.R., Environmental electron microscopy (ETEM) for catalysts with a closed E-cell with carbon windows. Ultramicroscopy 106, 503–507 (2006)
L.C. Gontard, L.Y. Chang, C.J.D. Hetherington, A.I. Kirkland, D. Ozkaya, R.E. Dunin-Borkowski, Aberration-corrected imaging of active sites on industrial catalyst nanoparticles. Ange. Chem. Int. Ed. 46, 3683–3685 (2007)
L. Hansen, J.B. Wagner, in Proceedings of the 12th European Congress on Electron Microscopy, (Brno, 2000) 537–538
P.L. Hansen, J.B. Wagner, S. Helveg, J.R. Rostrup-Nielsen, B.S. Clausen, H. Topsoe, Atom resolved imaging of dynamic shape changes in supported copper nanocrystals. Science 295, 2053 (2002)
T.W. Hansen, J.B. Wagner, P.L. Hansen, S. Dahl, H. Topsoe, C.J.H. Jacobson, Science 294, 1508–1510 (2001)
A.A. Herzing, C.J. Kiely, A.F. Carley, P. Landon, G.J. Hutchings, Identification of active gold nanoclusters on iron oxide supports for CO oxidation. Science 321, 1331–1335 (2008)
A.A. Herzing, M. Watanabe, J.K. Edwards, M. Conte, Z.R. Tang, G.J. Hutchings, C.J. Kiely, Energy dispersive X-ray spectroscopy of bimetallic nanoparticles in an aberration corrected scanning transmission electron microscope. Faraday Discussions, 138, 337–351 (2008)
S. Hillyard, J. Silcox, Detector geometry, thermal diffuse scattering and strain effects in ADF STEM imaging. Ultramicroscopy 58, 6–17 (1995)
T. Huang, T. Yu, S. Jhao, Weighting variation of water–gas shift in steam reforming of methane over supported Ni and Ni–Cu catalysts. Ind. Eng. Chem. Res. 45, 150–156 (2006)
W.J. Huang, B. Jiang, R.S. Sun, J.M. Zuo, Towards sub-Å atomic resolution electron diffraction imaging of metallic nanoclusters: A simulation study of experimental parameters and reconstruction algorithms. Ultramicroscopy 107, 1159–1170 (2007)
W.J. Huang, R. Sun, J. Tao, L.D. Menard, R.G. Nuzzo, J.M. Zuo, Coordination-dependent surface atomic contraction in nanocrystals revealed by coherent diffraction. Nat. Mater. 7, 308–313 (2008)
E. Iglesia, S.L. Soled, R.A. Fiato, G.H. Via, Bimetallic synergy in cobalt–ruthenium Fischer–Tropsch synthesis catalysts. J. Catal. 143, 345–368 (1993)
M. Inokuti, J.L. Dehmer, T. Baer, J.D. Hanson, Oscillator strength moments, stopping power and total inelastic scattering cross sections of all atoms through strontium. Phys. Rev. A 23, 95–109 (1981)
M.S. Isaacson, J. Langmore, N.W. Parker, D. Kopf, M. Utlaut, The study of the adsorption and diffusion of heavy atoms on light element substrates by means of the atomic resolution STEM. Ultramicroscopy 1, 359–376 (1976)
G. Jacobs, P.M. Patterson, Y. Zhang, T. Das, J. Li, B.H. Davis, Fischer–Tropsch synthesis: deactivation of noble metal-promoted Co/Al2O3 catalysts. Appl. Catal. A 233, 215–226 (2002)
J.S. Kim, T. LaGrange, B.W. Reed, M.L. Taheri, M.R. Armstrong, W.E. King, N.D. Browning, G.H. Campbell, Imaging of transient structures using nanosecond in situ TEM. Science 321, 1472–1475 (2008)
K. Kimoto, T. Asaka, T. Nagai, M. Saito, Y. Matsui, K. Ishizuka, Element-selective imaging of atomic columns in a crystal using STEM and EELS. Nature 450, 702–704 (2007)
E.J. Kirkland, Advanced Computing in Electron Microscopy (Plenum Press, New York, NY, 1998)
R.F. Klie, M.M. Disko, N.D. Browning, Atomic scale observations of the chemistry at the metal–oxide interface in heterogeneous catalysts. J. Catal. 205, 1–6 (2002)
A. Kogelbauer, J.G. Goodwin Jr., R. Oukaci, Ruthenium promotion of Co/Al2O3 Fischer–Tropsch catalysts. J. Catal. 160, 125–133 (1996)
K.T. Kohlmann, M. Thiemann, W.H. Brünger, E-beam induced X-ray mask repair with optimized gas nozzle geometry. Microelectron. Eng. 13, 279–282 (1991)
T.C. Lee, D.K. Dewald, J.A. Eades, I.M. Robertson, H.K. Birnbaum, An environmental cell transmission electron microscope. Rev. Sci. Instrum. 62, 1438–1444 (1991)
Y. Li, J. Chen, L. Chang, Y. Qin, The doping effect of copper on the catalytic growth of carbon fibers from methane over a Ni/Al2O3 catalysts prepared from Feitknecht compound precursor. J. Catal. 178, 76–83 (1998)
P. Li, J. Liu, N. Nag, P.A. Crozier, Atomic-scale study of in-situ metal nanoparticle synthesis in a Ni/TiO2 system. J. Chem. Phys. B 109, 13883–13890 (2005)
P. Li, J. Liu, N. Nag, P.A. Crozier, Dynamic nucleation and growth of Ni nanoparticles on high surface area titania. Surface Sci. 600, 693–702 (2006a)
P. Li, J. Liu, N. Nag, P.A. Crozier, In situ synthesis and characterization of Ru promoted Co/Al2O3 Fischer–Tropsch catalysts. Appl. Catal. A 307(2), 212–221 (2006b)
P. Li, J. Liu, N. Nag, P.A. Crozier, In situ preparation of Ni-Cu/TiO2 bimetallic catalysts. J. Catal. 262, 73–82 (2009)
Z.Y. Li, N.P. Young, M. DiVece, S. Palomba, R.E. Palmer, A.L. Bleloch, B.C. Curley, R.L. Johnson, J. Jiang, J. Juan, Three-dimensional atomic-scale structure of size-selected gold nanoclusters. Nature 451, 46–48 (2008)
J.Y. Liu, Advanced Electron Microscopy Characterization of Nanostructured Heterogeneous Catalysts, Microscopy and Microanalysis, 10, 55–76 (2004)
J.Y. Liu, Scanning transmission electron microscopy and its application to the study of nanoparticles and nanoparticle systems. J. Electron Microsc. 54, 251–278 (2005)
J. Liu, J.M. Cowley, High-angle ADF and high-resolution SE imaging of supported catalysts clusters. Ultramicroscopy 34, 119–128 (1990)
R.-J. Liu, P.A. Crozier, C.M. Smith, D.A. Hucul, J. Blackson, G. Salaita, In-situ electron microscopy studies of the sintering of palladium nanoparticles on alumina during catalyst regeneration processes. Microsc. Microanal. 10, 77–85 (2004)
R.-J. Liu, P.A. Crozier, C.M. Smith, D.A. Hucul, J. Blackson, G. Salaita, A new contact sintering mechanism associated with regeneration of Pd/Al2O3 hydrogenation catalyst. Appl. Catal. A 282, 111–121 (2005)
Y. Liu, D.Z. Liu, Study of bimetallic Cu–Ni/g-Al2O3 catalysts for carbon dioxide hydrogenation. Int. J. Hydrogen Energy 24, 351–354 (1999)
A.R. Lupini, S.J. Pennycook, Localization in elastic and inelastic scattering. Ultramicroscopy 96, 313–322 (2003)
C.E. Lyman, J.I. Goldstein, D.B. Williams, D.W. Ackland, S. von Harrach, N. A.W., P.J. Statham, High-performance X-ray detection in a new analytical electron microscope. J. Microsc. 176, 85–98 (1994)
C.E. Lyman, R.E. Lakis, H.G. Stenger, X-ray emission spectrometry of phase separation in Pt–Rh nanoparticles for nitric oxide reduction. Ultramicroscopy 58, 25–34 (1995)
C.E. Lyman, R.E. Lakis, H.G. Stenger Jr., B. Tøtdal, R. Prestvik, Analysis of alloy nanoparticles. Microchim. Acta 132, 301–308 (2000)
L. Marton, Bull. Acad. R. Belg. Cl. Sci 21, 553 (1935)
S. Matsui, T. Ichihashi, In situ observation on electron-beam-induced chemical vapor deposition by transmission electron microscopy. Appl. Phys. Lett. 53, 842–844 (1988)
L.D. Menard, F.T. Xu, R.G. Nuzzo, J.C. Yang, Preparation of TiO2-supported Au nanoparticle catalysts from a Au-13 cluster precursor: Ligand removal using ozone exposure versus a rapid thermal treatment. J. Catal. 243, 64–73 (2006)
P.A. Midgley, M. Weyland, 3D electron microscopy in the physical sciences: The development of Z-contrast and EFTEM tomography. Ultramicroscopy 96, 413–431 (2003)
K. Mitsuishi, M. Shimojo, M. Han, K. Furuya, Electron-beam-induced deposition using a subnanometer sized probe of high-energy electrons. Appl. Phys. Lett. 83, 2064–2066 (2003)
M. Mogensen, in Ceria-Based Electrodes. Catalysis by Ceria and Related Materials, ed. by A. Trovarelli (Imperial College Press, London, 2002), pp. 453–481
M. Mogensen, D. Lybye, N. Bonanos, P.V. Hendriksen, F.W. Poulsen, Factors controlling the oxide ion conductivity of fluorite and perovskite structured oxides. Solid State Ionics 174, 279–286 (2004)
M. Mogensen, N.M. Sammes, G.A. Tompsett, Physical, chemical and electrochemical properties of pure and doped ceria. Solid State Ionics 129, 63–94 (2000)
M.S. Moreno, M. Weyland, P.A. Midgley, J.F. Bengoa, M.V. Cagnoli, N.G. Gallegos, A.M. Alvarez, S.G. Marchetti, Highly anisotropic distribution of iron nanoparticles within MCM-41 mesoporous silica. Micron 37, 52–56 (2006)
D.A. Muller, L.F. Kourkoutis, M. Murfitt, J.H. Song, H.Y. Hwang, J. Silcox, N. Dellby, O.L. Krivanek, Atomic-scale chemical imaging of composition and bonding by aberration-corrected microscopy. Science 319, 1073–1076 (2008)
R. Naghash, T.H. Etsell, S. Xu, XRD and XPS study of Cu–Ni interactions on reduced copper–nickel–aluminum oxide solid solution catalyst. Chem. Mater. 18, 2480–2488 (2006)
R. Naghash, S. Xu, T.H. Etsell, Coprecipitation of nickel–copper–aluminum takovite as catalyst precursors for simultaneous production of carbon nanofibers and hydrogen. Chem. Mater. 17, 815–821 (2005)
P.D. Nellist, S.J. Pennycook, Direct imaging of the atomic configuration of ultradispersed catalysts. Science 274, 413–415 (1996)
P.D. Nellist, S.J. Pennycook, Incoherent imaging using dynamically scattered coherent electrons. Ultramicroscopy 78, 111–124 (1999)
N.L. Okamoto, B.W. Reed, S. Mehraeen, A. Kulkarni, D.G. Morgan, B.C. Gates, N.D. Browning, Determination of nanocluster sizes from dark-field scanning transmission electron microscopy images. J. Phys. Chem. C 112, 1759–1763 (2008)
V. Oleshko, P. Crozier, R. Cantrell, A. Westwood, In situ and ex situ study of propylene polymerization with a MgCl2-supported Ziegler-Natta catalyst. Stud. Surf. Sci. Catal. 130, 935–940 (2000)
V. Oleshko, P.A. Crozier, R. Cantrell, A. Westwood, In-situ real-time environmental TEM of gas phase Ziegler-Natta catalytic polymerization of propylene. J. Electron Microsc. 51(Suppl.), S27–S39 (2002)
V.P. Oleshko, P.A. Crozier, R.D. Cantrell, A.D. Westwood, In-situ and ex-situ study of gas phase propylene polymerization over a high activity TiCl4–MgCl2 heterogeneous Zeigler-Natta catalyst. Macromol. Rapid Commun. 22, 34–40 (2001)
M. Pan, J.M. Cowley, J.C. Barry, Coherent electron microdiffraction from small metal particles. Ultramicroscopy 30, 385–394 (1989)
M. Pan, J.M. Cowley, I.Y. Chan, Study of highly dispersed Pt in Y-zeolites by STEM and electron microdiffraction. Ultramicroscopy 34, 93–101 (1990)
G.M. Parkinson, Catal. Lett. 2, 303 (1989)
S.J. Pennycook, Study of supported ruthenium catalysts by STEM. J. Microsc. 124, 15–22 (1981)
S.J. Pennycook, D.E. Jesson, High-resolution incoherent imaging of crystals. Phys. Rev. Lett. 64, 938–941 (1990)
R. Prestvik, B. Tøtdal, C.E. Lyman, A. Holmen, Bimetallic particle formation in Pt–Re/Al2O3 reforming catalysts revealed by energy-dispersive X-Ray spectrometry in the analytical electron microscope. J. Catal. 176, 246–252 (1998)
W.D. Pyrz, D.A. Blom, N.R. Shiju, V.V. Guliants, T. Vogt, D.J. Buttrey, Using aberration-corrected STEM imaging to explore chemical and structural variations in the M1 phase of the MoVNbTeO oxidation catalyst. J. Phys. Chem. C 112, 10043–10049 (2008)
L. Reimer, Scanning Electron Microscopy (Springer-Verlag, Berlin, 1985)
S.B. Rice, S.A. Bradley, Imaging supported metal catalysts: the case for annular dark-field microscopy. Catal. Today 21, 71–82 (1994)
F.M. Ross, J. Tersoff, M.C. Reuter, Sawtooth faceting in silicon nanowires. Phys. Rev. Lett. 95, 4 (2005)
R. Sharma, P.A. Crozier, In situ electron microscopy of CeO2 and CeO2–ZrO2 reduction. Inst. Phys. Conf. Ser. 61, 569–572 (1999)
R. Sharma, P.A. Crozier, in Environmental Transmission Electron Microscopy in Nanotechnology Handbook of Microscopy for Nanotechnology, eds. by N. Yao, Z.L. Wang (Kluwer, New York, NY, 2005), pp. 531–563
R. Sharma, P.A. Crozier, Z.C. Kang, L. Eyring, Observation of dynamic nanostructural and nanochemical changes in ceria-based catalysts during in situ reduction. Philos. Mag. 84, 2731–2747 (2004)
R. Sharma, P.A. Crozier, R. Marx, K. Weiss, An environmental transmission electron microscope for in-situ observation of chemical processes at the nanometer level. Microsc. Microanal. 9(Suppl. 02), CD 912–913 (2003)
R. Sharma, Z. Iqbal, In situ observations of carbon nanotube formation using environmental transmission electron microscopy. Appl. Phys. Lett. 84, 990–992 (2004)
R. Sharma, E. Moore, P. Rez, M.M.J. Treacy, Site-specific fabrication of Fe particles for carbon nanotube growth. Nano Lett. 9, 689–694 (2009)
R. Sharma, K. Weiss, Microsc. Res. Tech. 42, 270–280 (1998)
M. Shelef, R.W. McCabe, Twenty-five years after introduction of automotive catalysts: what next? Catal. Today 62, 35–50 (2000)
A.J. Simoens, R.T.K. Baker, D.J. Dwyer, C.R.F. Lund, R.J. Madon, A study of the nickel–titanium oxide interaction. J. Catal. 86, 359–372 (1984)
S.B. Simonsen, S. Dahl, E. Johnson, S. Helveg, Ceria-catalyzed soot oxidation studied by environmental transmission electron microscopy. J. Catal. 255, 1–5 (2008)
J.H. Sinfelt, Catalysis by alloys and bimetallic clusters. Accounts Chem. Res. 10, 15–20 (1977)
A. Singhal, J.C. Yang, J.M. Gibson, STEM-based mass spectroscopy of supported Re clusters. Ultramicroscopy 67, 191 (1997)
K. Sohlberg, S. Rashkeev, A.Y. Borisevich, S.J. Pennycook, S.T. Pantelides, Origin of anomalous Pt–Pt distances in the Pt/alumina catalytic system. Chemphyschem 5(12), 1893–1897 (2004)
R.L. Stewart, Insulating films formed under electron and ion bombardment. Phys. Rev. 45, 488–490 (1934)
K. Sun, J. Liu, N. Nag, N.D. Browning, Studying the metal–support interaction in Pd/gamma-Al2O3 catalysts by atomic-resolution electron energy-loss spectroscopy. Catal. Lett. 84, 193–199 (2002a)
K. Sun, J. Liu, N.K. Nag, N.D. Browning, Atomic scale characterization of supported Pd–Cu/gamma-Al2O3 bimetallic catalysts. J. Phys. Chem. B 106, 12239–12246 (2002b)
K. Sun, J.Y. Liu, N.D. Browning, Direct atomic scale analysis of the distribution of Cu valence states in Cu/-gamma-Al2O3 catalysts. Appl. Catal. B Environ. 38, 271–281 (2002c)
P.R. Swann, N.J. Tighe, Proc. 5th Eur. Reg. Cong. Electron Microsc. 436 (1972)
K. Takeuchi, T. Matsuzaki, H. Arakawa, T. Hanaoka, Y. Sugi, Synthesis of C2-oxygenates from syngas over cobalt catalysts promoted by ruthenium and alkaline earths. Appl. Catal. A 48, 149–157 (1989)
B.L. Thiel, M. Toth, Secondary electron contrast in low-vacuum/environmental scanning electron microscopy of dielectrics. J. Appl. Phys. 97, 051101 (2005)
J.M. Thomas, P.L. Gai, Electron Microscopy and the Materials Chemistry of Solid Catalysts. Advances in Catalysis, vol. 48. (Elsevier, San Diego, 2004), pp. 171–227
M.M.J. Treacy, Imaging with Rutherford scattered electrons in the scanning transmission electron microscope. Scann. Electron Microsc. 1, 185–197 (1981)
M.M.J. Treacy, A. Howie, S.J. Pennycook, Z contrast of supported catalysts particles on the STEM. Inst. Phys. Conf. Ser. 52, 261–264 (1980)
M.M.J. Treacy, A. Howie, C.J. Wilson, Z-contrast of platinum and palladium catalysts. Philos. Mag. A 38, 569–585 (1978)
M.M.J. Treacy, S.B. Rice, Catalyst particle sizes from Rutherford scattered intensities. J. Microsc. 156, 211–234 (1989)
A. Trovarelli, Catalysis by Ceria and Related Materials (Imperial College Press, London, 2002)
B.H. Upton, C.C. Chen, N.M. Rodriguez, R.T.K. Baker, In situ electron microscopy studies of the interaction of iron, cobalt, and nickel with molybdenum disulfide single crystals in hydrogen. J. Catal. 141, 171–190 (1993)
J. van de Loosdrecht, M. van der Haar, A.M. van der Kraan, A.J. van Dillem, J.W. Geus, Preparation and properties of supported cobalt catalysts for Fischer–Tropsch synthesis. Appl. Catal. A 150, 365–376 (1997)
R.A. van Santen, J.W. Niemantsverdriet, Chemical Kinetics and Catalysis (Plenum Press, London, 1995)
R.A. van Santen, P.W.N.M. van Leeuwen, J.A. Moulijn, Catalysis: An Integrated Approach (Elsevier, Amsterdam, 1999)
M. Varela, S.D. Findlay, A.R. Lupini, H.M. Christen, A.Y. Borisevich, N. Dellby, O.L. Krivanek, P.D. Nellist, M.P. Oxley, L.J. Allen, S.J. Pennycook, Spectroscopic imaging of single atoms within a bulk solid. Phys. Rev. Lett. 92, 095502 (2004)
P.C.K. Vesborg, I. Chorkendorff, I. Knudsen, O. Balmes, J. Nerlov, A.M. Molenbroek, B.S. Clausen, S. Helveg, Transient behavior of Cu/ZnO-based methanol synthesis catalysts. J. Catal. 262, 65–72 (2009)
J. Wall, J. Langmore, M.S. Isaacson, A.V. Crewe, Scanning transmission electron microscopy at high resolution. Proc. Natl. Acad. Sci. 71, 1–5 (1974)
H. Wang, R.T.K. Baker, Decomposition of methane over a Ni–Cu–MgO catalyst to produce hydrogen and carbon nanofibers. J. Phys. Chem. B 108, 20273–20277 (2004)
R. Wang, P.A. Crozier, R. Sharma, J.B. Adams, Nanoscale heterogeneity in ceria zirconia with low-temperature redox properties. J. Phys. Chem. B 110, 18278–18285 (2006)
R. Wang, P.A. Crozier, R. Sharma, J.B. Adams, Measuring the redox activity of individual catalytic nanoparticles in cerium-based oxides. Nanoletters 8, 962–967 (2008)
S.W. Wang, A.Y. Borisevich, S.N. Rashkeev, M.V. Glazoff, K. Sohlberg, S.J. Pennycook, S.T. Pantelides, Dopants adsorbed as single atoms prevent degradation of catalysts. Nat. Mater. 3, 274–274 (2004)
M. Watanabe, D.W. Ackland, A. Burrows, C.J. Kiely, D.B. Williams, O.L. Krivanek, N. Dellby, M.F. Murfitt, Z. Szilagyi, Improvements in the X-Ray Analytical Capabilities of a Scanning Transmission Electron Microscope by Spherical-Aberration Correction. Microscopy and Microanalysis, 12, 515–526 (2006).
J.H.L. Watson, An effect of electron bombardment upon carbon black. J. Appl. Phys. 18, 153–161 (1947)
J.H.L. Watson, Specimen contamination in electron microscopes. J. Appl. Phys. 19, 110–111 (1948)
K. Wikander, A.B. Hungria, P.A. Midgley, A.E.C. Palmqvista, K. Holmberg, J.M. Thomas, Incorporation of platinum nanoparticles in ordered mesoporous carbon. J. Colloid Interf. Sci. 305, 204–208 (2007)
S. Wu, C. Zhu, W. Huang, Properties of polymer supported Ni–Cu bimetallic catalysts prepared by solvated metal atom impregnation. Chin. J. Polym. Sci. 14, 217–224 (1996)
M.J. Yacaman, J.A. Ascencio, S. Tehuacanero, M. Marin, Modem applications of electron microscopy to catalysis. Top. Catal. 18, 167–173 (2002)
J.C. Yang, S. Bradley, J.M. Gibson, The oblate morphology of supported PtRu5 on carbon black. Mater. Charact. 51, 101–107 (2003)
N. Yao, G.E. Spinnler, R.A. Kemp, D.C. Guthrie, R.D. Cates, C.M. Bolinger, Proceedings of the 49th Annual; Meeting of Microscopy Society of America, San Francisco Press, 1028–1029 (1991)
N.J. Zaluzec, Detector solid angle formulas for use in X-ray energy dispersive spectrometry. Microsc. Microanal. 15, 93–98 (2009)
Y. Zhang, D. Wei, S. Hammache, J.G. Goodwin Jr., Effect of water vapor on the reduction of Ru-promoted Co/Al2O3. J. Catal. 188, 281–290 (1999)
J.M. Zuo, M. Gao, J. Tao, B.Q. Li, R. Twesten, I. Petrov, Coherent nano-area electron diffraction. Microsc. Res. Tech. 64, 347–355 (2004)
Acknowledgements
I would like to thank colleagues and former students for contributions, collaborations and discussions over the years from many who have contributed to the work present in this chapter including Renu Sharma, Karl Weiss, Vladimir Oleshko, Peng Li, Ruigang Wang, Jingyue Liu and Nabin Nag. Financial support is acknowledged from Dow Chemical Company, Monsanto Company and the National Science Foundation (NSF-CTS-0306688 and NSF-CBET-0553445) and the Department of Energy for funding the ESTEM (DOE # AAD-0-30621-01). I also gratefully acknowledge access to the instrumentation in John M. Cowley Center for High Resolution Electron Microscopy in the LeRoy Eyring Center for Solid State Science at Arizona State University.
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Crozier, P.A. (2011). Nanocharacterization of Heterogeneous Catalysts by Ex Situ and In Situ STEM. In: Pennycook, S., Nellist, P. (eds) Scanning Transmission Electron Microscopy. Springer, New York, NY. https://doi.org/10.1007/978-1-4419-7200-2_13
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