CuFe2O4 spinel nanostructured were elaborated by mechanical alloying technique from Cu, Cu2O and Fe2O3 under controlled atmosphere with different milling times at room temperature. The CuFe2O4 spinel crystalline has a body‐centred tetragonal structure at low temperatures with lattice parameters a ≅ 0.582 nm and c ≅ 0.869 nm and face‐centred cubic structure at high temperatures with lattice parameter a ≅ 0.842 nm. The average crystallite size and lattice strain determined from X‐ray diffraction for CuFe2O4 are 22.12 ± 5.47 nm and 0.781 ± 0.082 %, respectively. The FTIR‐ATR spectra of the samples shows that the vibration around of 400–1000 cm−1 corresponds to the CuFe2O4 absorbed at octahedral and tetrahedral sites. The mechanical alloying process results in CuFe2O4 agglomerated in clusters, which radically change their shape during milling time. Differential scanning calorimetry analysis shows two additional endothermic peaks around 715–781 °C and 863–957 °C, the first peak might be affected to the formation of Cu‐Fe‐O and the second peak may correspond to the transformation of CuFe2O4 from tetragonal to cubic structure. CuFe2O4 samples milled until 20 h are ferromagnetic at room temperature with saturation magnetization increasing from 29.8 to 59.6 emu/g with increasing the milling time. The coercivity decreases 254 Oe up to 230 Oe when the milling time increases from 0 to 20h.