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Abstract  

A new method to measure heat flux and thermal expansion simultaneously with a temperature resolution of milli-Kelvin is presented to observe the multistage transitions. At least six thermal anomalies are observed between 402 and 403 K in BaTiO3 simultaneously in heat flux and thermal expansion in the cooling process. The correspondence of the anomalies observed in the two physical properties is excellent.

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Summary The size effect on the crystal structure including the chemical bonding nature has been investigated for several kinds of BaTiO3 nanopowder with the particle sizes down to 50 nm in diameter, by means of powder diffraction using high-energy synchrotron radiation. The Rietveld refinement reveals that the BaTiO3 nanopowder consists of tetragonal and cubic structure components at 300 K. The feature of coexistence can be illustrated by the core/shell model for the particle, in which the shell with a cubic structure covers the core with a tetragonal structure. The thickness of the cubic shell is almost constant irrespective of the particle sizes, and is estimated as approximately 8 nm. Hence, the critical particle-size, where the entire particle is covered with the cubic shell, is suggested as 16 nm. The charge density distributions of the BaTiO3 nanopowder in the cubic phase at 410 K are revealed by the maximum entropy method. Changes in the bonding electron density and the ionic valence expected are not observed clearly even in the 50 nm crystal compared with the bulk crystal.

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Abstract  

The changes of physico-chemical properties of mechanochemically pretreated (BaCO3 +TiO2 +PbO) powders were investigated. The values of apparent activation energy of BaTiO3 formation calculated by the Freeman and Carroll method decrease with milling time. The changes of precursors density may be interpreted as a consequence of mechanochemical reactions during milling.

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Journal of Thermal Analysis and Calorimetry
Authors: Adelina Ianculescu, Ana Brăileanu, M. Crişan, P. Budrugeac, N. Drăgan, G. Voicu, D. Crişan, and V. Marinescu

Abstract  

In order to obtain pure and fine BaTiO3 powders with controlled morphology, sol-precipitation methods involving the use of titanium iso-propoxide and of two different barium sources, i.e. barium nitrate and barium acetate, were proposed in this work. The thermal behaviour of the synthesized gels and the X-ray diffraction data obtained for the oxide powders pointed out that, by using Ba(NO3)2 as barium source, the decomposition process was completed at lower temperature (750C) and was accompanied by a more pronounced tendency to obtain a single phase BaTiO3 composition, by comparison with the synthesis where barium acetate was used as raw material (1100C). Scanning electron microscopy investigations emphasized the effect of the nature of barium source and synthesis conditions on the morphology of the oxide powders, as well as on the microstructure of the related ceramics.

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Abstract  

BaTiO3, was studied by positron lifetime spectroscopy in static electric fioeld. The strength of the field was varied from 0 up to 104 V/cm. Two characteristic points were found at 4500 V/cm and at 8500 V/cm. These field strengths were related to subsequent ordering processes of the crystal. Additional temperaturee dependent measurements were perforrmed in the 70–310 range to confirn the interopretaion of the two positron lifetimes. The two expected phase transitions were observed and these measurements showd that positron are trapped by Ba vacancies.

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Thermodynamic considerations of the grain size dependency of material properties

A new approach to explain the variation of the dielectric permittivity of BaTiO3 with grain size

Journal of Thermal Analysis and Calorimetry
Authors: P. Perriat, J. Niepce, and G. Caboche

Abstract  

Phase transitions which depend on grain size induce very interesting properties in materials such as zirconia or barium titanate. A new and rigorous thermodynamic treatment of this type of phase transition is proposed with consideration of the surface phenomena. An interpretation is given of the observed differences when the material—particularly BaTiO3—under consideration is a fine grain powder or is a fine grain ceramic.

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Abstract  

The crystal structures of BaTiO3 and PbTiO3 fine particles have been investigated by powder diffraction using synchrotron radiation high energy X-rays. It is revealed that a BaTiO3 fine particle essentially consists of tetragonal and cubic structure components at 300 K, whereas a PbTiO3 fine particle consists of a tetragonal structure. Adopting a structure model for the BaTiO3 particle that a cubic shell covers a tetragonal core, the thickness of cubic BaTiO3 shell is estimated at almost constant irrespective of particle sizes. Successive phase transitions are detected in 100 nm particles of BaTiO3 near the phase-transition temperatures of a bulk crystal. The changes in diffraction profiles are small, but they are apparent for a most up-to-date powder diffractometry.

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Abstract  

The SCTA method implies to control the temperature in such a way that the reaction rate changes with the time according to a function previously defined by the user. Constant Rate Thermal Analysis (CRTA) is one of the most commonly used SCTA methods and implies achieving a temperature profile at which the reaction rate remains constant all over the process at a value previously selected by the user. This method permits to minimize the influence of heat and mass transfer phenomena on the forward reaction. The scope of this work is to develop a universal CRTA temperature controller that could be adapted to any thermoanalytical device. The thermoanalytical signal is programmed to follow a preset linear trend by means of a conventional controller that at the time controls a second conventional temperature programmer that forces the temperature to change for achieving the trend programmed for the thermoanalytical signal. Examples of the performance of this control system with a Thermobalance and a Thermomechanical Analyser (TMA) are given.

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Abstract  

Matrix isolation of ferroelectric BaTiO3 nanoparticles was executed by formation of protective silica shell (via hydrolysis and polycondensation of tetraethyl orthosilicate) on particles of precursor—barium titanyl oxalate. Synthesized BaTiO3–SiO2 composites have been characterized by IR spectroscopy, XRD, TEM, DTA/DTG methods.

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Abstract  

Embedding of barium titanate into porous oxide matrices via sol–gel synthesis and introduction in structured slurry based on fumed oxides has been carried out. Prepared compositions have been studied using XRD, DTA-TG, FTIR, TEM, and adsorption of nitrogen. It has been established that simultaneous formation both barium titanate crystal structure and porous structure of matrices occurs. Crystallites of barium titanate, which arise in pores, possess lesser size in comparison with that for bulk BaTiO3.

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