Sinkler, W, Sanchez, SI, Bradley, SA et al. (4 more authors) (2015) Aberration-Corrected Transmission Electron Microscopy and In Situ XAFS Structural Characterization of Pt/γ-Al2O3 Nanoparticles. ChemCatChem, 7 (22). pp. 3779-3787. ISSN 1867-3880
Abstract
Aberration-corrected (AC) STEM, AC TEM and in situ X-ray absorption fine structure spectroscopy (XAFS) were used to characterize the Pt clusters present on a 0.35 wt % Pt on γ-alumina support after reduction in hydrogen at 700 °C. STEM high-angle annular dark field imaging shows that cluster formation takes place at temperatures up to approximately 350 °C, and this is followed by gradual growth in cluster size for heat treatments in hydrogen up to 700 °C. The STEM data show that after 700 °C reduction the Pt clusters are present in a narrow size distribution centered at 0.88 nm, and using a method involving a redistribution of the Pt atoms using a high electron dosage in the STEM, it is shown that the clusters are present in two-dimensional morphology. This conclusion is verified using intensity line scans. The in situ extended X-ray absorption fine structure data are in good agreement with these observations. High-resolution AC–TEM, which uses a broad coherent electron beam, and can thus offer advantages relative to STEM for structure determination of fine clusters, supported by image simulations of through-focus series, were used to analyze the structures of Pt particles. The structures determined by using AC–TEM are consistent with STEM and EXAFS data in having a flat two-dimensional morphology. Comparison of AC–STEM and AC TEM data for the same 700 °C reduced sample suggests that parallel-beam TEM mode of imaging may be advantageous because of the less pronounced beam-induced structural rearrangements that occur when imaging with a fine STEM probe.
Metadata
Item Type: | Article |
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Authors/Creators: |
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Keywords: | electron microscopy; nanostructu; platinum; supported catalysts; X-ray absorption spectroscopy |
Dates: |
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Institution: | The University of Leeds |
Academic Units: | The University of Leeds > Faculty of Engineering & Physical Sciences (Leeds) > School of Chemical & Process Engineering (Leeds) |
Depositing User: | Symplectic Publications |
Date Deposited: | 23 Feb 2018 15:35 |
Last Modified: | 23 Feb 2018 15:35 |
Status: | Published |
Publisher: | Wiley |
Identification Number: | 10.1002/cctc.201500784 |
Open Archives Initiative ID (OAI ID): | oai:eprints.whiterose.ac.uk:127221 |