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Microstructural and Defect Analysis of Metal Nanoparticles in Functional Catalysts by Diffraction and Electron Microscopy: The Cu/ZnO Catalyst for Methanol Synthesis

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Abstract

The application of different methods for a microstructural analysis of functional catalysts is reported for the example of different Cu/ZnO-based methanol synthesis catalysts. Transmission electron microscopy and diffraction were used as complementary techniques to extract information on the size and the defect concentration of the Cu nano-crystallites. The results, strengths and limitations of the two techniques and of different evaluation methods for line profile analysis of diffraction data including Rietveld-refinement, Scherrer- and (modified) Williamson–Hall-analyses, single peak deconvolution and whole powder pattern modeling are compared and critically discussed. It was found that in comparison with a macrocrystalline pure Cu sample, the catalysts were not only characterized by a smaller crystallite size, but also by a high concentration of lattice defects, in particular stacking faults. Neutron diffraction was introduced as a valuable tool for such analysis, because of the larger number of higher-order diffraction peaks that can be detected with this method. An attempt is reported to quantify the different types of defects for a selected catalyst.

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Authors and Affiliations

  1. Department of Inorganic Chemistry, Fritz-Haber-Institut der Max-Planck-Gesellschaft, Faradayweg 4-6, 14195, Berlin, Germany

    Timur Kandemir, Igor Kasatkin, Frank Girgsdies, Stefan Zander, Stefanie Kühl, Robert Schlögl & Malte Behrens

  2. Helmholtz-Zentrum Berlin, Hahn-Meitner-Platz 1, 14109, Berlin, Germany

    Michael Tovar

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  1. Timur Kandemir
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  2. Igor Kasatkin
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  4. Stefan Zander
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  5. Stefanie Kühl
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Correspondence to Robert Schlögl or Malte Behrens.

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Kandemir, T., Kasatkin, I., Girgsdies, F. et al. Microstructural and Defect Analysis of Metal Nanoparticles in Functional Catalysts by Diffraction and Electron Microscopy: The Cu/ZnO Catalyst for Methanol Synthesis. Top Catal 57, 188–206 (2014). https://doi.org/10.1007/s11244-013-0175-2

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