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A hybrid electrochemical–thermal method for the preparation of large ZnO nanoparticles

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Abstract

A simple and efficient two-step hybrid electrochemical–thermal route was developed for the synthesis of large quantity of ZnO nanoparticles using aqueous sodium bicarbonate electrolyte and sacrificial Zn anode and cathode in an undivided cell under galvanostatic mode at room temperature. The bath concentration and current density were varied from 30 to 120 mmol and 0.05 to 1.5 A/dm2. The electrochemically generated precursor was calcined for an hour at different range of temperature from 140 to 600 °C. The calcined samples were characterized by XRD, SEM/EDX, TEM, TG-DTA, FT-IR, and UV–Vis spectral methods. Rietveld refinement of X-ray data indicates that the calcined compound exhibits hexagonal (Wurtzite) structure with space group of P63mc (No. 186). The crystallite sizes were in the range of 22–75 nm based on Debye–Scherrer equation. The TEM results reveal that the particle sizes were in the order of 30–40 nm. The blue shift was noticed in UV–Vis absorption spectra, the band gaps were found to be 5.40–5.11 eV. Scanning electron micrographs suggest that all the samples were randomly oriented granular morphology.

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Acknowledgments

The authors thank to Kuvempu University Karnataka, India for providing the lab facilities to bring about this work, and also Department of Science and Technology (DST), New Delhi, Government of India (GOI) for providing financial support by Major Research Project (No. S.R/S3/ME/014/2007).

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Authors and Affiliations

  1. Department of P.G. Studies & Research in Chemistry, School of Chemical Sciences, Kuvempu University, Jnana Sahyadri Campus, Shankaraghatta, 577451, Karnataka, India

    Kodihalli G. Chandrappa, Thimmappa V. Venkatesha & Kanagalasara Vathsala

  2. Solid State and Structural Chemistry Unit, Indian Institute of Science, Bangalore, 560012, India

    Chikkadasappa Shivakumara

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  1. Kodihalli G. Chandrappa
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Correspondence to Thimmappa V. Venkatesha.

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Chandrappa, K.G., Venkatesha, T.V., Vathsala, K. et al. A hybrid electrochemical–thermal method for the preparation of large ZnO nanoparticles. J Nanopart Res 12, 2667–2678 (2010). https://doi.org/10.1007/s11051-009-9846-0

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