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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• 作者：Timur Kandemir (1)
  Igor Kasatkin (1)
  Frank Girgsdies (1)
  Stefan Zander (1)
  Stefanie Kühl (1)
  Michael Tovar (2)
  Robert Schl?gl (1)
  Malte Behrens (1)
  
• 关键词：Microstructure ; Defects ; Diffraction ; Electron microscopy ; Copper ; Methanol synthesis
• 刊名：Topics in Catalysis
• 出版年：2014
• 出版时间：February 2014
• 年：2014
• 卷：57
• 期：1-4
• 页码：188-206
• 全文大小：977 KB
• 作者单位：Timur Kandemir (1)
  Igor Kasatkin (1)
  Frank Girgsdies (1)
  Stefan Zander (1)
  Stefanie Kühl (1)
  Michael Tovar (2)
  Robert Schl?gl (1)
  Malte Behrens (1)
  
  1. Department of Inorganic Chemistry, Fritz-Haber-Institut der Max-Planck-Gesellschaft, Faradayweg 4-6, 14195, Berlin, Germany
  2. Helmholtz-Zentrum Berlin, Hahn-Meitner-Platz 1, 14109, Berlin, Germany
  
• ISSN：1572-9028

文摘

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.