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Synthesis of La-doped ceria nanoparticles: impact of lanthanum depletion

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Abstract

The present work explores the possible issues involving the synthesis of La-doped ceria-based nanoparticles by co-precipitation; moreover demonstrates the consequence of such issues in the final system. The stoichiometric anomaly as revealed by the X-ray diffraction (XRD) peak shift studies confirmed a massive departure from the final target composition; indicating lanthanum depletion (~30 %) from the resultant oxide. This also revealed that a fraction of this unreacted lanthanum precursor stayed in the system alone. Transmission electron microscopy results revealed the presence of nanocrystalline La-oxycarbonate phase as a fine dispersion co-existing with the lanthanum cerate nanocrystals; XRD could not detect the presence of such a phase at 550 °C. Through Raman and Fourier transform infrared spectroscopy analyses, a possible pathway of this complex thermal transition for the free La-precursor was outlined (100–1200 °C). The Raman data unambiguously pointed out the transition zone for the decomposition sequence for its conversion from La-nitrate to oxycarbonate in the temperature range 400–550 °C. The overall study emphasises the need of special attention for synthesising La-based solid solution systems via colloidal routes; especially considering the solubility and mixing issues for the lanthanum precursor.

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Acknowledgments

The authors thank Prof. Goutam Deo, Department of Chemical Engineering, Indian Institute of Technology Kanpur for the Raman Spectroscopy experiments. Kushal Singh gratefully acknowledges the financial supports provided by Indian Institute of Technology Patna.

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Correspondence to Anirban Chowdhury.

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Singh, K., Kumar, R. & Chowdhury, A. Synthesis of La-doped ceria nanoparticles: impact of lanthanum depletion. J Mater Sci 51, 4134–4141 (2016). https://doi.org/10.1007/s10853-016-9736-7

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  • DOI: https://doi.org/10.1007/s10853-016-9736-7

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