Study of the formation of the apatite- type phases La9.33+x(SiO4)(6)O2+3x/2 synthesized from a lanthanum oxycarbonate La2O2CO3

摘要

Lanthanum silicated apatites with nominal composition La9.33+x(SiO4)(6)O2+3x/2 (-0.2 < x < 0.27) have been successfully synthesized by solid state reaction using a new reagent La2O2CO3 and amorphous SiO2 precursors. The formation mechanism of La2O2CO3 reagent, which cannot be purchased, has been followed by in-situ temperature depend XRD of La2O3 under CO2 atmosphere. The stability of this reagent during the synthesis step allowed to limit the formation of secondary phase La2Si2O7 and made the weighting of the reagent easier. High purity powders could be synthesized at the temperature of 1400 degrees C. Dense pellets (more than 98.5%) were obtained by isostatic pressing of powders calcined at 1200 degrees C and then sintered at 1550 degrees C. Traces of La2SiO5 secondary phase present in synthesized powder disappeared after densification and pure oxyapatite materials were obtained for all the compositions. Electrical measurements confirmed that conductivity behaviors of the sintered pellets were dependent to the oxygen over-stoichiometry. Indeed, a relatively high conductivity of 1 x 10(-2) S cm(-1) was exhibited at 800 degrees C for the nominal composition La-9.60(SiO4)(6)O-2.405 with low activation energy around 0.79 eV. The ionic conductivity properties were comparable with that of the earlier obtained materials. (C) 2014 Elsevier Masson SAS. All rights reserved.