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BaTiO3 formation by thermal decomposition of a (BaTi)-citrate polyester resin in air

Published online by Cambridge University Press:  31 January 2011

P. Durán ,
F. Capel ,
J. Tartaj  and
C. Moure
P. Durán
Affiliation:
Instituto de Ceraámica y Vidrio (CSIC), Electroceramics Department, 28500-Arganda del Rey, Madrid, Spain
F. Capel
Affiliation:
Instituto de Ceraámica y Vidrio (CSIC), Electroceramics Department, 28500-Arganda del Rey, Madrid, Spain
J. Tartaj
Affiliation:
Instituto de Ceraámica y Vidrio (CSIC), Electroceramics Department, 28500-Arganda del Rey, Madrid, Spain
C. Moure
Affiliation:
Instituto de Ceraámica y Vidrio (CSIC), Electroceramics Department, 28500-Arganda del Rey, Madrid, Spain
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Abstract

Barium titanate nanosized powders were prepared by a slightly modified Pechini method. The obtained polymerized resin was used as the precursor for BaTiO3 powder production. DTA TG thermal analysis indicated that thermal decomposition of the precursors proceeds through four major step processes: (i) dehydration reaction; (ii) combustion reactions; (iii) intermediate phases formation; (iv) decarbonation of the intermediate to give BaTiO3. X-ray diffractometry (XRD) and Raman spectroscopy results indicated that, depending on the heating rate, the BaTiO3 formation took place via a predominant solid-state reaction between nanosized BaCO3 and amorphous TiO2 (TiO2−x) when crystallized by a low-heating rate (1.5 °C/min), although a small amount of a quasi-amorphous intermediate phase was also present. BaTiO3 crystallization by rapid heating rate (5 °C/min) took place through a quasi-amorphous intermediate phase formation as the main rate-controlling factor for the crystallization process. The fact that the low heating rate minimizes the intermediate phase content indicates the strong influence of the thermal heating on the kinetics of the involved transformation or in the mechanism. Although XRD results seem to indicate the formation of pseudocubic BaTiO3 as the final reaction product, the Raman spectra indicated as more probable the formation of a mixture of an oxygen-deficient hexagonal and tetragonal BaTiO3 phases below 700 °C. Above that temperature the tetragonal BaTiO3 was the only phase present. As-prepared BaTiO3 strongly agglomerated powders were relatively sinter active, leading to dense ceramic bodies (≥95% of the theoretical value). Microstructural (grain size approximately 1 mm) and room-temperature dielectric properties (ετ ≈ 2000 and tan δ ≤ 2%) at 10 kHz indicated that the obtained powders have to be optimized.

Type
Articles
Information
Journal of Materials Research , Volume 16 , Issue 1 , January 2001 , pp. 197 - 209
Copyright
Copyright © Materials Research Society 2001

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