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Microsc Microanal. 2014 Jun;20(3):982-90. doi: 10.1017/S1431927614000373. Epub 2014 Mar 18.

Tomographic heating holder for in situ TEM: study of Pt/C and PtPd/Al2O3 catalysts as a function of temperature.

Microscopy and microanalysis : the official journal of Microscopy Society of America, Microbeam Analysis Society, Microscopical Society of Canada

Lionel C Gontard, Rafal E Dunin-Borkowski, Asunción Fernández, Dogan Ozkaya, Takeshi Kasama

Affiliations

  1. 1Instituto de Ciencia de Materiales de Sevilla (CSIC),41092,Sevilla,Spain.
  2. 2Ernst Ruska-Centre for Microscopy and Spectroscopy with Electrons (ER-C) and Peter Grünberg Institute (PGI),Forschungszentrum Jülich,D-52425 Jülich,Germany.
  3. 3Johnson Matthey Technology Centre,Blount's Court,Sonning Common,Reading RG4 9NH,UK.
  4. 4Center for Electron Nanoscopy,Technical University of Denmark,DK-2800 Kgs. Lyngby,Denmark.

PMID: 24641835 DOI: 10.1017/S1431927614000373

Abstract

A tomographic heating holder for transmission electron microscopy that can be used to study supported catalysts at temperatures of up to ~1,500°C is described. The specimen is placed in direct thermal contact with a tungsten filament that is oriented perpendicular to the axis of the holder without using a support film, allowing tomographic image acquisition at high specimen tilt angles with minimum optical shadowing. We use the holder to illustrate the evolution of the active phases of Pt nanoparticles on carbon black and PtPd nanoparticles on γ-alumina with temperature. Particle size distributions and changes in active surface area are quantified from tilt series of images acquired after subjecting the specimens to increasing temperatures. The porosity of the alumina support and the sintering mechanisms of the catalysts are shown to depend on distance from the heating filament.

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