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Structural and chemical characterization of SnO2-based nanoparticles as electrode material in Li-ion batteries

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Abstract

Improvement of long-term stability of electrode materials in Li-ion batteries requires a detailed understanding of influence of synthesis parameters on surface chemistry and on properties. Therefore, bare SnO2 and core/shell nanoparticles with SnO2 core and a hydrocarbon shell are synthesized in an Ar/20% O2 microwave plasma, deposited as porous nanoparticle films in situ on heated Ni-substrates, and finally assembled as anodes in Swagelok cells. In a comprehensive study, we investigate structure, particle size, chemistry, morphology, and water content of the nanoparticles using X-ray diffraction, transmission electron microscopy, specific surface area analysis, and coulometric water titration. The thicknesses of the nanoparticle films and their surface chemistry are investigated by scanning electron microscopy and X-ray photoelectron spectroscopy. SnO2 nanoparticles are crystalline, with a tetragonal cassiterite structure. Primary particle sizes around 3 nm are reached for the bare SnO2 particles, 5–8 nm for the cores of the core/shell nanoparticles. A minimum microwave power of 900 W is necessary to synthesize SnO2 nanoparticles without precursor residuals as pristine SnO2 particles for the subsequent coating step. In the coating step increasing hydrocarbon content can be correlated with increasing carbon-precursor feeding rate. Water uptake, stemming either from the process, or due to atmospheric contamination, can successfully be reduced by a thermal treatment. The still remaining water is a function of specific surface area. Finally, bare SnO2 versus core/shell nanoparticles are compared regarding the influence of the shell on the electrochemical properties. The principal improved functionality of the developed anodes in Swagelok cells is demonstrated.

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Acknowledgements

The authors acknowledge financial support by the German Ministry for Education and Research, project “Battery Competence Consortium South—Electrochemistry for Electromobility” under contract number 03KP801.

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Authors and Affiliations

  1. Institute of Applied Materials – Materials Process Technology, Karlsruhe Institute of Technology, Hermann-von-Helmholtz-Platz 1, 76344, Eggenstein-Leopoldshafen, Germany

    Dorothée Vinga Szabó, Goran Kilibarda, Sabine Schlabach, Vanessa Trouillet & Michael Bruns

  2. Department of Microsystems Engineering, Albert-Ludwigs-University of Freiburg, Georges-Koehler-Allee 102, 79110, Freiburg, Germany

    Goran Kilibarda

Authors
  1. Dorothée Vinga Szabó
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  2. Goran Kilibarda
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  3. Sabine Schlabach
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Correspondence to Dorothée Vinga Szabó.

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Szabó, D.V., Kilibarda, G., Schlabach, S. et al. Structural and chemical characterization of SnO2-based nanoparticles as electrode material in Li-ion batteries. J Mater Sci 47, 4383–4391 (2012). https://doi.org/10.1007/s10853-012-6292-7

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