ChemCatChem

Cover image for Vol. 5 Issue 9

Special Issue: Advanced Microscopy for Catalysis

September 2013

Volume 5, Issue 9

Pages 2541–2723

  1. Cover Pictures

    1. Top of page
    2. Cover Pictures
    3. Editorial
    4. Graphical Abstract
    5. News
    6. Essay
    7. Communications
    8. Full Papers
    1. You have free access to this content
      Cover Picture: Optimum Energy-Dispersive X-Ray Spectroscopy Elemental Mapping for Advanced Catalytic Materials (ChemCatChem 9/2013) (page 2541)

      Dr. Bingsen Zhang, Dr. Wei Zhang, Dr. Lidong Shao and Prof. Dr. Dang Sheng Su

      Article first published online: 27 AUG 2013 | DOI: 10.1002/cctc.201390042

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      Cartography for the catalysis researcher The cover picture shows that the observation of individual elements in advanced catalytic materials can be achieved by determining optimum conditions for obtaining an accurate STEM-EDX elemental map. In their Communication on p. 2586 ff., D. S. Su et al. reveal that a suitable combination of dwell time and beam intensity is crucial in pinpointing elemental distribution by using STEM-EDX mapping. Importantly, trace amounts of catalytic species can be observed towards the analytical limit to determine information, such as elemental composition, size, and morphology, as well as, in particular, the possible dynamic changes in nanoparticles after catalytic reactions.

    2. You have free access to this content
      Inside Cover: Revealing the Atomic Structure of Intermetallic GaPd2 Nanocatalysts by using Aberration-Corrected Scanning Transmission Electron Microscopy (ChemCatChem 9/2013) (page 2542)

      Rowan Leary, Dr. Francisco de la Peña, Dr. Jonathan S. Barnard, Yuan Luo, Dr. Marc Armbrüster, Prof. Sir John Meurig Thomas and Prof. Paul A. Midgley

      Article first published online: 27 AUG 2013 | DOI: 10.1002/cctc.201390043

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      Up close and personal with nanocatalysts The cover picture shows the generation of a false-color image of GaPd2. In their Full Paper on p. 2599 ff., R. Leary et al. describe the atomic structure of GaPd2 nanocatalysts by using aberration-corrected STEM (AC-STEM) and annular dark-field imaging. AC-STEM provided direct insight into the distinct structure and chemical ordering of the intermetallic phase GaPd2 in nanosized particles. It also revealed deviations from the ideal “bulk” structure. The study highlights the importance of considering nanoparticle morphologies and nanocrystalline defects.

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      Inside Back Cover: Strong Metal–Support Interaction: Growth of Individual Carbon Nanofibers from Amorphous Carbon Interacting with an Electron Beam (ChemCatChem 9/2013) (page 2999)

      Dr. Wei Zhang and Dr. Luise Theil Kuhn

      Article first published online: 27 AUG 2013 | DOI: 10.1002/cctc.201390046

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      Nanofibers on the rise! The cover picture shows that individual carbon nanofibers can by grown from a mixture of amorphous carbon and Ce0.8Gd0.2O1.9/Ni nanoparticles by using an electron beam in a 300 kV transmission electron microscope, without any gaseous carbon source, and external heating. In their Communication on p. 2591 ff., W. Zhang and L. T. Kuhn demonstrate that an electron beam can bridge physical mixing to chemical bonding in a designed porosity. The induced strong metal-support interaction effect can result in a local arrangement of carbon atoms in the amorphous carbon.

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      Back Cover: Microstructural Analysis and Energy-Filtered TEM Imaging to Investigate the Structure–Activity Relationship in Fischer–Tropsch Catalysts (ChemCatChem 9/2013) (page 3000)

      Dr. Ileana Florea, Yuefeng Liu, Prof. Ovidiu Ersen, Dr. Christian Meny and Dr. Cuong Pham-Huu

      Article first published online: 27 AUG 2013 | DOI: 10.1002/cctc.201390047

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      Mapping the way for cobalt catalysis The cover picture shows a typical 3D montage of the analytical 3D model of a selected supported cobalt grain obtained by using energy filtered (EFTEM) tomographic analysis applied to Si, Ti, and Co elements. In their Full Paper on p. 2610 ff., O. Ersen, C. Pham-Huu et al. present a detailed analysis of their Co/TiO2-SiC catalyst by 2D and 3D chemical imaging, based on EFTEM, combined with the more traditional high-resolution TEM mode. The study allowed them to precisely solve the microstructure, the porous characteristics, and the distribution of the constituting phases.

  2. Editorial

    1. Top of page
    2. Cover Pictures
    3. Editorial
    4. Graphical Abstract
    5. News
    6. Essay
    7. Communications
    8. Full Papers
    1. You have free access to this content
      Special Issue: Advanced Electron Microscopy for Catalysis (pages 2543–2545)

      Prof. Dang Sheng Su

      Article first published online: 27 AUG 2013 | DOI: 10.1002/cctc.201300657

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      Up close and personal with catalysts: A great selection of advanced microscopy and analysis techniques are collated in this Special Issue. The attention to the finest detail of catalysis has never been more apparent or accessible and herein the Guest Editor, Prof. Dang Sheng Su, brings his introduction.

  3. Graphical Abstract

    1. Top of page
    2. Cover Pictures
    3. Editorial
    4. Graphical Abstract
    5. News
    6. Essay
    7. Communications
    8. Full Papers
    1. Graphical Abstract: ChemCatChem 9/2013 (pages 2547–2552)

      Article first published online: 27 AUG 2013 | DOI: 10.1002/cctc.201390044

  4. News

    1. Top of page
    2. Cover Pictures
    3. Editorial
    4. Graphical Abstract
    5. News
    6. Essay
    7. Communications
    8. Full Papers
  5. Essay

    1. Top of page
    2. Cover Pictures
    3. Editorial
    4. Graphical Abstract
    5. News
    6. Essay
    7. Communications
    8. Full Papers
    1. Some Turning Points in the Chemical Electron Microscopic Study of Heterogeneous Catalysts (pages 2560–2579)

      Prof. Sir John Meurig Thomas, Dr. Caterina Ducati, Rowan Leary and Prof. Paul A. Midgley

      Article first published online: 25 APR 2013 | DOI: 10.1002/cctc.201200883

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      Half a century, take a bow to the pavilion: Over the past 50 years or so, electron microscopy has become an invaluable technique for the study of solid catalysts. We recount some of the most important developments, including early high-resolution studies, insights obtained using aberration- corrected optics, recent advances in electron tomography, time-resolved electron microscopy, and precession electron diffraction.

  6. Communications

    1. Top of page
    2. Cover Pictures
    3. Editorial
    4. Graphical Abstract
    5. News
    6. Essay
    7. Communications
    8. Full Papers
    1. Clothing Carbon Nanotubes with Palladium Rings: Constructing Carbon[BOND]Metal Hybrid Nanostructures under Electron-Beam Irradiation (pages 2581–2585)

      Dr. Bingsen Zhang, Dr. Lidong Shao, Dr. Wei Zhang and Prof. Dr. Dang Sheng Su

      Article first published online: 5 JUN 2013 | DOI: 10.1002/cctc.201300249

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      What not to wear: This work illustrates the clothing of 1 D carbon nanotubes at desired locations with nanoengineered metal nanostructures in a ring pattern for nanodevice applications, such as catalysis.

    2. Optimum Energy-Dispersive X-Ray Spectroscopy Elemental Mapping for Advanced Catalytic Materials (pages 2586–2590)

      Dr. Bingsen Zhang, Dr. Wei Zhang, Dr. Lidong Shao and Prof. Dr. Dang Sheng Su

      Article first published online: 11 JAN 2013 | DOI: 10.1002/cctc.201200654

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      EDX marks the spot: STEM-EDX mapping is a highly useful tool for studying advanced catalytic materials. Beam intensity and dwell time can be adjusted to an optimum balance for obtaining an unambiguous elemental map.

    3. Strong Metal–Support Interaction: Growth of Individual Carbon Nanofibers from Amorphous Carbon Interacting with an Electron Beam (pages 2591–2594)

      Dr. Wei Zhang and Dr. Luise Theil Kuhn

      Article first published online: 12 JUL 2013 | DOI: 10.1002/cctc.201300452

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      To bridge physical mixing to chemical bonding? Use an electron beam! Individual carbon nanofibers can grow from physical mixing of amorphous carbon and Ce0.8Gd0.2O1.9/Ni nanoparticles, under an electron beam in a 300 kV transmission electron microscope, without any gaseous carbon source and external heating, as a consequence of strong metal support interaction effect occurring in the mixtures.

    4. Atomic Resolution Analysis of Microporous Titanosilicate ETS-10 through Aberration Corrected STEM Imaging (pages 2595–2598)

      Dr. Alvaro Mayoral, Prof. Joaquin Coronas, Dr. Clara Casado, Dr. Carlos Tellez and Dr. Isabel Díaz

      Article first published online: 4 APR 2013 | DOI: 10.1002/cctc.201300045

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      It′s all your fault! Microporous titanosilicate ETS-10 crystals have been analyzed by advanced electron microscopy techniques. With the last generation of spherical aberration corrected electron microscopes, truly atomic resolution images have been recorded. Owing to the extremely high-resolution images that have been obtained, the multiple defects (stacking faults, lack of porosity and “double-pores”) present in this type of material can be analyzed in great detail.

  7. Full Papers

    1. Top of page
    2. Cover Pictures
    3. Editorial
    4. Graphical Abstract
    5. News
    6. Essay
    7. Communications
    8. Full Papers
    1. Revealing the Atomic Structure of Intermetallic GaPd2 Nanocatalysts by using Aberration-Corrected Scanning Transmission Electron Microscopy (pages 2599–2609)

      Rowan Leary, Dr. Francisco de la Peña, Dr. Jonathan S. Barnard, Yuan Luo, Dr. Marc Armbrüster, Prof. Sir John Meurig Thomas and Prof. Paul A. Midgley

      Article first published online: 29 APR 2013 | DOI: 10.1002/cctc.201300029

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      A clear view in a dark field: The annular dark–field imaging mode and electron energy-loss spectroscopy were used to provide directly-interpretable imaging and chemical analysis of GaPd2 nanocatalysts, revealing intricacies of the “nano-sized” intermetallic compound that are intriguing from both a crystallographic and catalytic perspective.

    2. Microstructural Analysis and Energy-Filtered TEM Imaging to Investigate the Structure–Activity Relationship in Fischer–Tropsch Catalysts (pages 2610–2620)

      Dr. Ileana Florea, Yuefeng Liu, Prof. Ovidiu Ersen, Dr. Christian Meny and Dr. Cuong Pham-Huu

      Article first published online: 11 JUN 2013 | DOI: 10.1002/cctc.201300103

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      Secrets of the grain: Chemical imaging based on energy-filtered TEM in 2 D and 3 D (see picture) modes of Co/TiO2–SiC catalysts reveal that TiO2 doping is almost homogenous within the bimodal porous structure of β-SiC; small Co nanoparticles are found on TiO2 and larger ones are close to SiC. Co/TiO2–SiC catalysts are more active and stable in the Fischer–Tropsch synthesis than Co/SiC.

    3. Electrospun Metal Oxide Nanofibres for the Assessment of Catalyst Morphological Stability under Harsh Reaction Conditions (pages 2621–2626)

      Christian H. Kanzler, Sven Urban, Katarzyna Zalewska-Wierzbicka, Franziska Hess, Dr. Stefan F. Rohrlack, Claas Wessel, Dr. Rainer Ostermann, Dr. Jan P. Hofmann, Prof. Dr. Bernd M. Smarsly and Prof. Dr. Herbert Over

      Article first published online: 5 JUN 2013 | DOI: 10.1002/cctc.201300301

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      Spinning a tale of two cities: Electrospun RuO2- and CeO2-based nanofibers (NFs) are used as model catalysts to assess morphological stability of these materials under harsh HCl oxidation reaction conditions. For instance, RuO2 NFs are morphologically unstable, whereas mixed RuO2-TiO2 NFs are stable at 573 K. Thus, the use of NFs can serve as a general approach for the analysis of stability issues during the early stage of catalyst screening.

    4. Time Evolution of the Stability and Oxygen Reduction Reaction Activity of PtCu/C Nanoparticles (pages 2627–2635)

      Chinnaya Jeyabharathi, Dr. Nejc Hodnik, Claudio Baldizzone, Josef C. Meier, Dr. Marc Heggen, Dr. Kanala L. N. Phani, Dr. Marjan Bele, Milena Zorko, Dr. Stanko Hocevar and Dr. Karl J. J. Mayrhofer

      Article first published online: 5 JUL 2013 | DOI: 10.1002/cctc.201300287

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      Spheres of change: Electrochemical dealloying under potentiodynamic conditions induces changes from spherical to more cuboctahedral core–shell structures for particles in a size range of 10–20 nm. In contrast, during dealloying under potentiostatic conditions the semispherical shape of small particles is completely retained and extensive porosity is formed on all particles larger than 20 nm, as can be observed from identical location electron microscopy.

    5. Microstructure of Bimetallic Pt[BOND]Pd Catalysts under Oxidizing Conditions (pages 2636–2645)

      Tyne R. Johns, Dr. Jason R. Gaudet, Eric J. Peterson, Dr. Jeffrey T. Miller, Dr. Eric A. Stach, Dr. Chang H. Kim, Michael P. Balogh and Prof. Abhaya K. Datye

      Article first published online: 2 JUL 2013 | DOI: 10.1002/cctc.201300181

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      Structured learning: A comparison of the evolution of aged and aged-plus-reduced Pt, Pd, and bimetallic Pt[BOND]Pd particles is reported. The bimetallic particles grow in size and both Pt and Pd stay metallic in the form of large particles with a portion of Pd present as a dispersed Pd phase.

    6. Enhanced Photocatalytic Activity: Macroporous Electrospun Mats of Mesoporous Au/TiO2 Nanofibers (pages 2646–2654)

      Dr. Xingdong Wang, Dr. Jonghyun Choi, Dr. David R. G. Mitchell, Dr. Yen B. Truong, Dr. Ilias L. Kyratzis and Assoc. Prof. Rachel A. Caruso

      Article first published online: 5 JUN 2013 | DOI: 10.1002/cctc.201300180

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      Electrospinning top! A facile one-pot synthesis that couples electrospinning and sol–gel chemistry is used to form porous titania nanofibrous mats that contain gold nanoparticles. The enhanced photocatalytic activity of the products is because of the high crystallinity of the anatase phase, high porosity and surface area, and small gold nanoparticles (13±3 nm) within these samples.

    7. In Situ Aberration-Corrected Environmental TEM: Reduction of Model Co3O4 in H2 at the Atomic Level (pages 2655–2661)

      Michael R. Ward, Prof. Edward D. Boyes and Prof. Pratibha L. Gai

      Article first published online: 3 JUN 2013 | DOI: 10.1002/cctc.201300047

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      Co3O4 reduction is CoOl: By using advanced aberration-corrected environmental TEM, the intricacies of the dynamic atomic scale reduction of Co3O4 in H2 that are of interest in hydrogenation reactions, such as the Fischer–Tropsch process, have been investigated. Notably, at low pressure the transformation proceeds via an advancing interface between Co3O4 and CoO regions. Co metal is observed at higher pressure.

    8. Atomic-Scale Probing the Priority of Oxidation Sites of an Organic Molecule Adsorbed at the Cu[BOND]O/Cu(1 1 0) Interface (pages 2662–2666)

      Kai Sheng, Huihui Kong, Zhiwen Li, Chi Zhang, Qiang Sun, Dr. Qinggang Tan, Dr. Yunxiang Pan, Prof. Dr. Aiguo Hu and Prof. Dr. Wei Xu

      Article first published online: 22 FEB 2013 | DOI: 10.1002/cctc.201200955

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      Adsorbent with four binding modes: The interface between metal and oxides is considered to play a key role in redox reactions. A combination of STM imaging and DFT calculations provided direct evidence at the atomic scale that the interface of Cu[BOND]O/Cu(1 1 0) is the most favorable site for the adsorption and activation of an organic, multifunctional molecule.

    9. Light-Induced Reduction of Cuprous Oxide in an Environmental Transmission Electron Microscope (pages 2667–2672)

      Filippo Cavalca, Dr. Anders B. Laursen, Dr. Jakob B. Wagner, Christian D. Damsgaard, Prof. Dr. Ib Chorkendorff and Dr. Thomas W. Hansen

      Article first published online: 10 APR 2013 | DOI: 10.1002/cctc.201200887

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      Illuminating photocatalysis: Exposing cuprous oxide to light in an aqueous environment causes reduction to metallic copper. Using a combination of imaging, diffraction, and spectroscopy new insights into the reduction mechanism have been obtained.

    10. Quantitative Z-Contrast Imaging of Supported Metal Complexes and Clusters—A Gateway to Understanding Catalysis on the Atomic Scale (pages 2673–2683)

      Dr. Nigel D. Browning, Dr. Ceren Aydin, Dr. Jing Lu, Dr. Apoorva Kulkarni, Dr. Norihiko L. Okamoto, Prof. Volkan Ortalan, Dr. Bryan W. Reed, Dr. Alper Uzun and Prof. Bruce C. Gates

      Article first published online: 20 MAR 2013 | DOI: 10.1002/cctc.201200872

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      Pinpointing catalytic sites:­ Z-contrast imaging in an aberration-corrected scanning transmission electron microscope is used to reveal the size, shape, and composition of supported metal complexes. In tandem with spectroscopic techniques, the structure of these complexes can be fully resolved on the atomic scale.

    11. An Atomic Scale View of Methanol Reactivity at the Cu(1 1 1)/CuOx Interface (pages 2684–2690)

      Timothy J. Lawton, Dr. Georgios Kyriakou, Dr. Ashleigh E. Baber and Prof. E. Charles H. Sykes

      Article first published online: 6 MAR 2013 | DOI: 10.1002/cctc.201200810

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      Methanol all around the perimeter: The interaction and reaction of methanol on a catalytically relevant Cu/CuOx interface has been studied at the atomic scale with scanning tunneling microscopy.

    12. Ni-Catalyzed Growth of Graphene Layers during Thermal Annealing: Implications for the Synthesis of Carbon-Supported Pt[BOND]Ni Fuel-Cell Catalysts (pages 2691–2694)

      Dr. Lin Gan, Stefan Rudi, Dr. Chunhua Cui and Prof. Dr. Peter Strasser

      Article first published online: 23 JUL 2013 | DOI: 10.1002/cctc.201300235

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      Layer cake: The solid-state transformation of a carbon support into graphene-like layers was achieved during the thermal annealing of carbon-supported PtxNi1–x catalysts with higher Ni content. In turn, the resultant instability of the carbon support promoted particle migration and coalescence, thus leading to more-significant particle sintering on Ni-richer PtxNi1–x catalysts.

    13. A Study of Commercial Nanoparticulate γ-Al2O3 Catalyst Supports (pages 2695–2706)

      Yahaya Rozita, Prof. Rik Brydson, Dr. Tim P. Comyn, Dr. Andrew J. Scott, Dr. Chris Hammond, Dr. Andy Brown, Sandra Chauruka, Dr. Ali Hassanpour, Dr. Neil P. Young, Prof. Angus I. Kirkland, Dr. Hidetaka Sawada and Dr. Ron I. Smith

      Article first published online: 24 APR 2013 | DOI: 10.1002/cctc.201200880

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      New insights into familiar supports: We investigate a range of commercially available γ-Al2O3 powders by using a combination of integrated experimental techniques such as XRD, neutron powder diffraction, and TEM. Most of the γ-Al2O3 powders studied comprised a significant proportion of cubeoctahedral nanoparticles containing numerous steps on the {1 1 1}-type aluminum cation-rich surface facets.

    14. Surface Segregation of Pd from TiO2-Supported AuPd Nanoalloys under CO Oxidation Conditions Observed In situ by ETEM and DRIFTS (pages 2707–2716)

      Dr. Laurent Delannoy, Prof. Suzanne Giorgio, Dr. Jean Gabriel Mattei, Dr. Claude R. Henry, Dr. Nadia El Kolli, Dr. Christophe Méthivier and Dr. Catherine Louis

      Article first published online: 7 FEB 2013 | DOI: 10.1002/cctc.201200618

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      Gold Ghost in the Shell: Surface Pd segregation is observed upon exposure of bimetallic AuPd nanoparticles to a CO+O2 reaction mixture. The process was scrutinized by means of two in situ techniques, environmental high-resolution electron microscopy (ETEM) and diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS).

    15. Carbon-Supported Gold Nanocatalysts: Shape Effect in the Selective Glycerol Oxidation (pages 2717–2723)

      Dr. Di Wang, Dr. Alberto Villa, Dr. Dangsheng Su, Prof. Laura Prati and Prof. Robert Schlögl

      Article first published online: 30 NOV 2012 | DOI: 10.1002/cctc.201200535

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      Order, order! More ordered graphitic layers on the supporting carbon nanofibers surface led to Au particles bonded through their {1 1 1} plane, exhibiting more facet area. This catalyst presented higher selectivity toward C[BOND]C bond cleavage in the liquid-phase oxidation of glycerol.

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