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Large-scale electrochemical synthesis of SnO2 nanoparticles

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Abstract

Tin oxide nanoparticles were synthesized by electrochemical oxidation of a tin metal sheet in a non-aqueous electrolyte containing NH4F. The as-prepared nanoparticles were then thermally annealed at 700 °C for 6 h. The resulting particles were characterized by a variety of experimental techniques, including X-ray diffraction (XRD), high-resolution transmission electron microscopy (HRTEM), Raman, UV-visible, and photoluminescence (PL) spectroscopy. The XRD patterns clearly showed that the amorphous phase of the as-synthesized SnO2 particles was transformed into a rutile-type crystalline structure after thermal treatment; and from the line broadening of the XRD peaks, the average size of the annealed particles was found to be 15.4, 12.5, 11.8 nm for the particles initially synthesized at 20, 30, and 40 V, respectively. Consistent results were also observed in HRTEM measurements which showed clear crystalline lattice fringes of the calcined nanoparticles, as compared to the featureless profiles of the as-produced counterparts. In Raman spectroscopic studies, three dominant peaks were observed at 480, 640, and 780 cm−1 which were ascribed to the E1g, A1g, and B2g Raman active vibration modes, respectively, and the wavenumbers of these peaks blue-shifted with decreasing particle size. Additionally, a broad strong emission band was observed in room-temperature photoluminescence measurements.

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Acknowledgements

This work was supported in part by the National Science Foundation (CHE-0718170 and DMR-0804049). The powder X-ray diffraction data in this work were recorded on an instrument supported by the NSF Major Research Instrumentation (MRI) Program under Grant No. CHE-0521569. We thank the National Center for Electron Microscopy at Lawrence Berkeley National Laboratory for use of its facilities. We also thank Prof. J. Z. Zhang, T. Olson and R. Newhouse (UCSC) for access to the Raman spectrometer, and Prof. S. Oliver and D. Rogow (UCSC) for assistance in XRD data acquisition.

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  1. Department of Chemistry and Biochemistry, University of California, 1156 High Street, Santa Cruz, CA, 95064, USA

    Wei Chen, Debraj Ghosh & Shaowei Chen

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  1. Wei Chen
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Chen, W., Ghosh, D. & Chen, S. Large-scale electrochemical synthesis of SnO2 nanoparticles. J Mater Sci 43, 5291–5299 (2008). https://doi.org/10.1007/s10853-008-2792-x

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