Nickel–aluminium and magnesium–aluminium hydrotalcites were prepared by co-precipitation and subsequently submitted to calcination. The mixed oxides obtained from the thermal decomposition of the synthesized materials were characterized by XRD, H₂-TPR, N₂ sorption and elemental analysis and subsequently tested in the reaction of methane dry reforming (DRM) in the presence of excess of methane (CH₄/CO₂/Ar=2/1/7). DMR in the presence of the nickel-containing hydrotalcite-derived material showed CH₄ and CO₂ conversions of ca. 50% at 550°C. The high values of the H₂/CO molar ratio indicate that at 550°C methane decomposition was strongly influencing the DRM process. The sample reduced at 900°C showed better catalytic performance than the sample activated at 550°C. The catalytic performance in isothermal conditions from 550°C to 750°C was also determined.