In the process of dry reforming of methane (DRM), the activity of low-percentage catalysts based on cobalt and iron oxides and their modification with nickel oxide was studied. It has been established that the addition of nickel oxide into the Fe2O3/γ-Al2O3 catalyst increases the degree of methane conversion from 14 to 89%, and also increases the yield of target reaction products H2 to 43.0 vol.%, CO to 46.1 vol.% at 850 °C. On a Co3О4-NiО/γ-Al2O3 catalyst at 850 °C, methane conversion reaches to 88.1%, the yield of H2 and CO is 44.8%. TPR-H2 analyzes showed that the introduction of nickel oxide into Fe2O3/γ-Al2O3 composition, in contrast to the Co3O4/γ-Al2O3 catalyst, the temperature peaks of Fe2O3-NiО/γ-Al2O3, reduction shift towards lower temperatures and weaken the interaction of metals with the support - γ-Al2O3 and thereby the amount of active reduced particles of iron and nickel oxides increases, which ensures good catalytic activity of Fe2O3-NiО/γ-Al2O3. According to the XRD results, spinel-like form - NiFe2O4, NiAl2O4 and CoAl2O4, also phase as Fe2O3 were obtained on the Fe2O3-NiО/γ-Al2O3 catalyst. This indicates that the developed catalysts form new phases that are active at high temperatures to produce synthesis gas in reduction-oxidation processes during the DRM reaction.