Thermal decomposition of the coordination polymer, (NH 4 (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. Perovskite-type oxides comprising lanthanide (f-elements) and d-transition metal ions, and related mixed oxides have been extensively studied for their practical uses as electrode materials in the solid oxide fuel cells, 1),2) gas sensors, 3),4) catalysts,oxygen permeable membranes 10) and platinum-free alkaline water electrolysis cells. 11) For preparing such perovskite-type oxides, solid state reaction and co-precipitation methods have been widely adopted. In the solid state reaction, metal oxides or metal carbonates as the components are mechanically mixed and calcined at high temperature (usually above 1273 K). In this reaction, the product is inevitably contaminated by the respective metal oxides of the component metals, and calcining and grinding are, in most cases, repeated for diminishing such contaminants. In the co-precipitation method, a contrivance is often needed for preparing homogeneous precipitates, because each component metal ion has its characteristic precipitation kinetics. In order to overcome these problems, various preparation methods have been developed. Among these, citrate process 7),12) and polymerizable complex method 13)15) are known to be effective for preparing nanoparticles of perovskite-type oxide single phase at relatively low temperature. Besides these methods, we have proposed the complex decomposition method which is based on thermal decomposition of heteronuclear complexes or coordination polymers isolated in advance. ¹1 at a heating rate of 10 K·min ¹1 from room temperature to 1273 K. FT-IR spectra were measured at room temperature with a JASCO V-4100 spectrometer. Powder X-ray diffraction (XRD) analyses were carried out at room temperature