P. Pinceloup et al., Hydrothermal synthesis of nanometer-sized barium titanate powders: Controlof barium/titanium ratio, sintering, and dielectric properties, J AM CERAM, 82(11), 1999, pp. 3049-3056
Nanometer-sized BaTiO3 powders have been synthesized hydrothermally from Ba
(OH)(2) and titanium alkoxide at 150 degrees C for 2 h, and the Ba/Ti ratio
has been measured with an accuracy of +/-0.003. Stoichiometric powders can
be obtained by adjusting the Ba/Ti ratio of the reactants to a value of 1.
018. At a lower Ba/Ti ratio, the solubility of Ba(OH)(2) prevents full inco
rporation of barium, and barium-deficient powders result. A higher Ba/Ti ra
tio leads to the incorporation of excess barium in the powder, K-s(BaTiO3,
-25 degrees C) = 7 x 10(-8) has been calculated for the equilibrium reactio
n. From this result, two reproducible processes for the synthesis of stoich
iometric BaTiO3 are proposed, The processes rely only on very accurate cont
rol of the chemical composition (Ba/Ti ratio) of the precursor suspension.
The sintering behavior of powders having Ba/Ti ratio values between 0.965 a
nd 1.011 is described from results of dilatometric measurements and isother
mal sintering, Room-temperature dielectric constants as high as 5600 and lo
sses as low as 0.009 have been obtained for a stoichiometry slightly less t
han 1.000. It is expected that optimum sintering behavior and electrical pr
operties are obtained in the stoichiometry range 0.995-1.000.