Journal of Materials Science, Vol.37, No.18, 4029-4039, 2002
Thermal decomposition of lanthanum-titanium citric complexes prepared from ethylene glycol medium
The paper addresses the thermal decomposition of La-, Ti- and bimetallic La-Ti-non-crystalline citric complexes, prepared in ethylene glycol medium. The latter complex is the starting material for the effective ferroelectric La2Ti2O7 preparation by the polymerized complex method. Based on thermogravimetric analysis (DTG, DTA and TG) and identification of some of the intermediates (by elemental analysis, NMR and IR spectroscopy and X-ray diffractometry), it is established that the thermal destruction proceeds step-wise, starting with dehydration above 50-60degreesC, partial transformation of the citrate to aconitate up to 200degreesC, followed by releasing of the ethylene glycol bonded as adduct and ester (200-280degreesC) and decarboxilation (280-335degreesC). The complete destruction of the organic components results in mixed-metal oxocarbonate. The process is completed at similar to750degreesC giving poorly crystalline La2Ti2O7. The results obtained are compared with those for a water-prepared NH4-La-Ti-citric complex.