Аннотация:A series of K2NiF4-like complex oxides Nd2-xCaxNiO4 (x = 0–0.4) was obtained by the freeze drying synthesis method. Thermal decomposition of these precursors in H2 at 900 oC resulted in the formation of Ni/(Nd2O3,CaO) composites with different Nd2O3/CaO ratios. Their microstructure was similar to the products of the redox exsolution of perovskites: spherical 30 nm particles of Ni metal were allocated at the surface of dense agglomerates of Nd2O3 and CaO grains. The as-obtained composites demonstrated significant catalytic activity, selectivity, and stability in the reactions of dry reforming and partial oxidation of methane (DRM and POM,respectively) at T >= 800 oC.