A new, less‐material‐intensive, and fast protocol was developed to synthesize NiFe2O4 spinel from hematite α‐Fe2O3. This is a solid state reaction at relatively low severity and short milling time (2–10 min). The product was characterized by X‐ray diffraction (XRD), scanning electron microscopy coupled with energy dispersive X‐ray spectroscopy, temperature‐programmed reduction, thermogravimetric analysis, and BET specific surface area.The produced NiFe2O4 was tested as a methane dry reforming catalyst (CH4 + CO2) to compare its activity with similar Ni‐Fe spinels reported in the literature.XRD revealed that under stoichiometric conditions, the resulting formulation contains only pure NiFe2O4, in a crystalline spinel structure. The catalytic performance of NiFe2O4 during CH4 dry reforming, at 800 °C for 4 h and a stoichiometric molar ratio of CO2/CH4 = 1, is described by the following results: CH4 conversion rose to about 40 % after 30 min over time‐on‐stream (TOS), then decreased more slowly to 25 % after 4 h of TOS. Over the same period, hydrogen (H2) yield increased to 50 % during the first 1 h of TOS, then following the same pattern as CH4 conversion, it dropped to 30 % over the next 4 h of TOS. These results show that the tested NiFe2O4 is better than those reported in the literature for similar catalytic use of nanometric NiFe2O4.