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A Study on the Polymer Precursor Formation and Microstructure Evolution of Square-Shaped (La0.5Ba0.5)(Mn0.5Fe0.5)O3 Ceramic Nanoparticles
M. Romero1,2, H. Pardo1,2, R. Faccio1,2, L. Suescun1,2, S. Vázquez1, I. Laborda1, L. Fernández-Werner1,2, Á. Acosta3, J. Castiglioni4, Á.W. Mombrú1,2
1 Cryssmat-Lab/Centro NanoMat – DETEMA – Facultad de Química – Universidad de la República – P.O. Box 1157, Montevideo, URUGUAY.
2 Centro Interdisciplinario de Nanotecnología, Química y Física de Materiales – Espacio Interdisciplinario – Universidad de la República – P.O. Box 1157, Montevideo, URUGUAY.
3 Cátedra de Química Inorgánica, DEC, Facultad de Química, Universidad de la República – P.O. Box 1157, Montevideo, URUGUAY.
4 Cátedra de Fisicoquímica, DETEMA, Facultad de Química, Universidad de la República – P.O. Box 1157, Montevideo, URUGUAY.
received January 23, 2015, received in revised form March 1, 2015, accepted March 10, 2015
Vol. 6, No. 3, Pages 221-230 DOI: 10.4416/JCST2015-00005
Abstract
The polymer precursor formation and the growth mechanism of (La0.5Ba0.5)(Mn0.5Fe0.5)O3 ceramic nanoparticles have been studied. First, we focused on the influence of isolated metals (La, Ba, Mn, Fe) on the polymer precursor formation by means of Raman, FT-IR, scanning electron microscopy and differential scanning calorimetry, showing that the presence of metal ions, especially iron, increases the oxidation rate of the polymer precursor, while the presence of barium leads to a higher degree of polymerization, preventing partial oxidation of the polymer at low temperatures and allowing the presence of nitrates at the combustion stage. Nevertheless, when all metals are present, the polymer precursor showed a largely homogeneous microstructure with a global average influence from all cations.
Finally, we studied the microstructure evolution of nanoparticles obtained after calcination above 700 °C. SAXS and TEM analysis suggests that the formation of square-shaped nanoparticles below 900 °C and coalescence leads to the formation of larger-sized and round-shaped nanoparticles at 900 °C.
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Keywords
SAXS, perovskite, nanoparticle, sol-gel, polymer precursor.
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