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Particle-shape control and formation mechanisms of hydrothermally derived lead titanate

Published online by Cambridge University Press:  31 January 2011

Jooho Moon ,
Melanie L. Carasso ,
Henrik G. Krarup ,
Jeffrey A. Kerchner  and
James H. Adair
Jooho Moon
Affiliation:
Department of Materials Science and Engineering, University of Florida, Gainesville, Florida 32611
Melanie L. Carasso
Affiliation:
Department of Materials Science and Engineering, University of Florida, Gainesville, Florida 32611
Henrik G. Krarup
Affiliation:
Department of Materials Science and Engineering, University of Florida, Gainesville, Florida 32611
Jeffrey A. Kerchner
Affiliation:
Department of Materials Science and Engineering, University of Florida, Gainesville, Florida 32611
James H. Adair
Affiliation:
Department of Materials Science and Engineering, University of Florida, Gainesville, Florida 32611
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Abstract

Phase-pure perovskite lead titanate with various morphologies has been synthesized by a hydrothermal method at 150 °C. Particle shapes include cubic, tabular, and aggregated platelike shapes. The feedstock concentration greatly influences particle morphology of the hydrothermally derived PbTiO3. At a concentration of 0.05 M, the tabular particles form while cubic particles are produced at 0.1 M. Aggregated plateletlike particles are synthesized at 0.125 M. It was observed that both tabular and cubic particles directly precipitate from the coprecipitated precursor gel. In contrast, the plateletlike shaped intermediate phase appears during the initial stage of reaction at 0.125 M and in situ transforms into perovskite PbTiO3 during further hydrothermal treatment. The intermediate phase preserves its particle shape during transformation and, acting as a template, gives rise to the final tabular PbTiO3 particles. It is demonstrated that only base reagents such KOH and NaOH, which provide a highly basic condition (i.e., pH > 14), promote transformation of the coprecipitated gel into the perovskite PbTiO3. A Hancock and Sharp kinetic analysis in conjunction with microstructural evidence suggests that the formation mechanism is dissolution and recrystallization in which the degree of supersaturation plays an important role in dictating the crystallographic particle phase and morphology of the particles. An experimentally constructed solubility diagram indicates that an excess lead condition is necessary to compensate for loss of lead species and to increase supersaturation to expedite precipitation of PbTiO3 at highly alkaline conditions.

Type
Articles
Information
Journal of Materials Research , Volume 14 , Issue 3 , March 1999 , pp. 866 - 875
Copyright
Copyright © Materials Research Society 1999

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