The mixed oxide LaNiO3 with perovskite structure was prepared by two relatively new and unconventional methods including preparation and thermal decomposition of mixed metal oxalate or carbonate precursors. The intermediates were prepared by reaction in a highly concentrated suspension (paste). The thermal decomposition conditions of these intermediates were described and the final calcination temperatures were determined, which was done using thermal analysis methods and X-ray diffraction. During the decomposition of mixed carbonates, one-phase LaNiO3 is produced directly, in case of decomposition of oxalates, a mixture of LaNiO3 and La2O3 is produced due to the formation of La2O2CO3 during the heating. Catalytic decomposition of nitrous oxide at high temperature (650 -930 °C) and high loading (GHSV = 350 000 h -1 ) has shown high LaNiO3 activity, even at lower temperatures. The results were compared with the same compound obtained by co-precipitation and by solid state reaction. Methods of preparation based on decomposition of oxalate and carbonate intermediates lead to the preparation of materials with appropriate composition, morphology, specific surface and high catalytic activity.