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Crystal microstructure of annealed nanocrystalline Chromium studied by synchrotron radiation diffraction

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Abstract

The microstructure of electrodeposited nanocrystalline chromium (n-Cr) was studied by using synchrotron radiation (SR) diffraction, SEM, TEM, and EDX techniques. The as-prepared n-Cr samples show the standard bcc crystal structure of Cr with volume-averaged column lengths varying from 25 to 30 nm. The grain growth kinetics and the oxidation kinetics were studied by time resolved SR diffraction measurements with n-Cr samples annealed at 400, 600, and 800 °C. The grain growth process is relatively fast and it occurs within the first 10 min of annealing. The final crystallite size depends only on the annealing temperature and not on the initial grain size or on the oxygen content. The final volume-averaged column lengths observed after 50 min annealing are 40(4), 80(1), and 120(2) nm for temperatures 400, 600, and 800 °C, respectively. It is shown that annealing ex situ of n-Cr at 800 °C both under vacuum and in air gives a grain growth process with the same final crystallite sizes. The formation of the Cr2O3 and CrH phases is observed during annealing.

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Acknowledgements

Thanks are due to Sylvia Kuhn and to Dr. Holger Kohlmann (both University of Saarbrücken) for their assistance with TEM, EDX investigations and with the vacuum annealing, respectively. Thanks are due to Iraida Snigireva (ESRF) for help with SEM investigations. One of the authors (DW) thanks the ESRF for support of his stay. The access to the ESRF facilities has been supported by the Ministry of Science and Higher Education (Poland) 155/ESR/2006/03.

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Author notes

  1. M. Bukowski

    Present address: Leibniz-Institut für Neue Materialien GmbH, D-66123, Saarbrücken, Germany

Authors and Affiliations

  1. Institute of Experimental Physics, Faculty of Physics, University of Warsaw, Hoża 69, 00-681, Warsaw, Poland

    D. Wardecki & R. Przeniosło

  2. European Synchrotron Radiation Facility, BP 220, F-38043, Grenoble Cedex, France

    A. N. Fitch

  3. Institute of Physical Chemistry, University of Saarland, D66123, Saarbrücken, Germany

    M. Bukowski & R. Hempelmann

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  1. D. Wardecki
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  2. R. Przeniosło
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  3. A. N. Fitch
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  4. M. Bukowski
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  5. R. Hempelmann
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Correspondence to D. Wardecki.

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Wardecki, D., Przeniosło, R., Fitch, A.N. et al. Crystal microstructure of annealed nanocrystalline Chromium studied by synchrotron radiation diffraction. J Nanopart Res 13, 1151–1161 (2011). https://doi.org/10.1007/s11051-010-0107-z

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