Abstract. NiFeCO3 hydrotalcites with Ni/Fe molar ratio of 3were synthesized by co-precipitationmethod at constant pH, followed by hydrothermal treatment at various temperatures 85–180 ◦C for 3–360 h. The obtained materials were characterized by XRD analysis, FT-IR spectroscopy, SEM and TEM microscopy, TGA and BET techniques. The resulting materials were found to be similar to the hydr…