A new, less-material-intensive, and fast protocol was developed to synthesize NiFe2O3 spinel from hematite alpha-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 NiFe2O3 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 crystalline only pure NiFe2O3, in a crystalline spinel structure. The catalytic performance of NiFe2O3 during CH4 dry reforming, at 800 degrees 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 (TOS), then decreased more slowly to 25 9 after 4 h of TOS. Over the same period, hydrogen (H-2) 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.