Microstructural and Defect Analysis of Metal Nanoparticles in Functional Catalysts by Diffraction and Electron Microscopy: The Cu/ZnO Catalyst for Methanol Synthesis. Kandemir, T., Kasatkin, I., Girgsdies, F., Zander, S., Kuehl, S., Tovar, M., Schloegl, R., & Behrens, M. Topics in Catalysis, 57(1-4):188–206, February, 2014. WOS:000330829600019
doi  abstract   bibtex   
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.
@article{kandemir_microstructural_2014,
	title = {Microstructural and {Defect} {Analysis} of {Metal} {Nanoparticles} in {Functional} {Catalysts} by {Diffraction} and {Electron} {Microscopy}: {The} {Cu}/{ZnO} {Catalyst} for {Methanol} {Synthesis}},
	volume = {57},
	issn = {1022-5528},
	shorttitle = {Microstructural and {Defect} {Analysis} of {Metal} {Nanoparticles} in {Functional} {Catalysts} by {Diffraction} and {Electron} {Microscopy}},
	doi = {10.1007/s11244-013-0175-2},
	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.},
	language = {English},
	number = {1-4},
	journal = {Topics in Catalysis},
	author = {Kandemir, Timur and Kasatkin, Igor and Girgsdies, Frank and Zander, Stefan and Kuehl, Stefanie and Tovar, Michael and Schloegl, Robert and Behrens, Malte},
	month = feb,
	year = {2014},
	note = {WOS:000330829600019},
	keywords = {Copper, Electron microscopy, Methanol synthesis, Stacking, crystallite size, defects, diffraction, dislocation contrast, lattice strain, line-broadening analysis, microstructure, powder diffraction, profile   analysis, x-ray-diffraction, zinc-oxide},
	pages = {188--206},
}

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