The preparation of nanometer γ-Fe2O3 through an electrochemical process was studied at room temperature, using a metal iron plate as sacrificing anode and a sheet of stainless steel as cathode, in non-aqueous mediate containing ( Bu)4 NBr as support electrolyte and 2 % (vol % ) water. The powdery particles obtained were then calcined at 300 ℃. The products were characterized by IR, XRD,SEM, TEM and laser particle size analyser, indicating the fine particle is a pure nanometer γ-Fe2O3. The morphology is like coneshaped and their average size is 22.0 nm. Furthermore the VSM spectrum shows that the particle's coercivity (3.9 × 103 A/m) is rather small, presenting the excellent super-paramagnetism.