H. Langbein et G. Wolki, PREPARATION OF COPPER NIOBATES BY THERMAL-DECOMPOSITION OF FREEZE-DRIED COMPLEX OXALATE SOLUTIONS, Thermochimica acta, 264, 1995, pp. 67-73
Freeze-dried complex oxalates of copper and niobium are reactive precu
rsors for ternary copper niobium oxides. The thermal decomposition of
the amorphous precursors has been investigated by DTA, TG and mass spe
ctroscopy. The gaseous decomposition products are assigned to steps in
the TG graph. Above 500 degrees C, crystallization of complex oxides
takes place. In the temperature range up to 900 degrees C, only the te
rnary phases CuNb2O6 and Cu3Nb2O8 can be synthesized. The thermal deco
mposition of the oxalate precursor is advantageous with regard to the
preparation of pure monoclinic CuNb2O6. The transformation between mon
oclinic and orthorhombic CuNb2O6 is reversible with a high activation
energy of transformation.