H. Fjellvag et al., THERMAL-ANALYSIS AS AN AID IN THE SYNTHESIS OF NONSTOICHIOMETRIC PEROVSKITE-TYPE OXIDES, Thermochimica acta, 256(1), 1995, pp. 75-89
The controlled synthesis of non-stoichiometric perovskite type oxides
is of importance for fundamental and applied studies. The present cont
ribution focuses on how data from thermal analysis, mainly thermogravi
metry and X-ray powder diffraction, can be utilized for defining optim
um synthesis conditions. The perovskite oxides frequently have (or are
formed from binary oxides with) high stability and low reactivity. Th
e synthesis of a homogeneous and pure reaction product is limited by d
iffusion controlled mass transport, and precursor materials with mixin
g of cations on a microscopic level are therefore needed. The decompos
ition of citrate precursors, the formation and decomposition of interm
ediates, the control of oxygen non-stoichiometry, the decomposition of
the product and reactions/phase transitions on cooling are considered
. As examples, thermal analysis data are provided and discussed for ma
jor steps in the syntheses of non-stoichiometric LaMO(3) (M is V, Cr,
Mn, Fe, Co or Ni).