Thermal decomposition of the coordination polymer, (NH
4)La[Fe
II(CN)
6]·4.5H
2O, with a three-dimensional network structure formed by the Fe
II–CN–La
III linkages, was investigated. The decomposition began at around 323 K and proceeded via a few steps to give the anhydride complex, (NH
4)La[Fe
II(CN)
6], at around 523 K. Further heating gave rise to an abrupt collapse of cyanide groups at around 573 K, followed by the initial formation of the perovskite-type oxide, LaFeO
3, at 603 K and the completion of the decomposition to produce LaFeO
3 at around 898 K. Any formation of the component metal oxides, La
2O
3 and Fe
2O
3, was not recognized during the decomposition. From the XRD line broadening using Scherrer’s equation, the average size of the thermal decomposition product was evaluated to be 21, 22, 25 and 30 nm at 773, 823, 898 and 1073 K, respectively. The specific surface area of the LaFeO
3 particles prepared at 898, 1073 and 1273 K was 13.2, 8.6 and 2.5 m
2 g
−1, respectively.
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