Environmental electron microscopy (ETEM) for catalysts with a closed E-cell with carbon windows

CRMCN1, CNRS, Campus de Luminy, Case 913, 13288 Marseille, Cedex 9, France.
Ultramicroscopy (Impact Factor: 2.75). 05/2006; 106(6):503-7. DOI: 10.1016/j.ultramic.2006.01.006
Source: PubMed

ABSTRACT In a standard high-resolution electron microscope (Jeol 3010), an environmental sample holder designed by Jeol, has been used for in situ observations at the atomic scale of catalysts, during a chemical reaction. Experiments have been performed in H(2) and O(2) at a pressure up to 4 mbar at room temperature, and in the case of H(2), at various temperatures until 350 degrees C. For the first time, Au and Pd clusters supported on TiO(2) and amorphous carbon have been observed with a windows-cell environmental electron microscopy (ETEM) system, with the resolution of the (1 1 1) lattice fringes. Au clusters have been cleaned in H(2) and have got the equilibrium shape of the fcc crystals during annealing. The same Au particles can be observed during successive treatments under O(2) and H(2). For Pd clusters in situ exposed to O(2) , the adhesion has decreased.

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    ABSTRACT: Atomic resolution has been obtained using environmental transmission electron microscopy (ETEM) by installing a spherical aberration corrector (Cs-corrector) on the objective lens. Simultaneously, the technology for controlling the environment around a specimen in ETEM has advanced significantly in the past decade. Quantification methodology has recently been established for deriving relevant experimental data in catalyst materials from substantial and systematic ETEM observation at the atomic scale. With this background, this paper summarizes aspects of the evolutional microscopy technique: necessary conditions for atomic resolution in ETEM; reduction of the scattering of electrons by the medium surrounding a specimen; and an environmental cell for structural imaging of a crystalline specimen. The high spatial resolution of a Cs-corrected ETEM is demonstrated for different observation conditions. After statistical analysis combined with numerical image analysis of ETEM data is briefly described, the recent applications of the Cs-corrected ETEM to catalyst materials are reviewed. For gold nanoparticulate catalysts, the structural information on the reaction sites and adsorption sites are deduced. For Pt nanoparticulate catalysts, ETEM studies elucidate the correlation between the catalytic activity and the morphology of the nanoparticles. These studies also reveal oxidation and reduction on the topmost Pt surface layer at the atomic scale. Finally, current issues and the future perspectives of Cs-corrected ETEM are summarized, including the reproducibility of ETEM observation data, the control of environments, the critical evaluation of electron irradiation effects, the full implementation of transmission electron microscopy technology in ETEM, and the safety issues for an ETEM laboratory. Copyright © 2014 Elsevier B.V. All rights reserved.
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