Mesoporous　ZnFe2O4　was　successfully　synthesized　through　the　reaction　of　Zn2+,　Fe2+　and　C2O42-　using　sodium　dodecyl　sulfate　(SDS)　as　size-controlling　reagent.　The　characterizations　were　done　by　X-ray　powder　diffraction　(XRD),　differential　thermal　analysis-thermo　gravimetric　analysis　(DTA-TG),　fourier　transform-infrared　spectroscopy　(FT-IR),　field　emission　scanning　electronic　microscopy　(FE-SEM),　nitrogen　adsorption-desorption　measurement,　showing　that　mesoporous　ZnFe2O4　can　be　obtained　after　calcined　at　500°C　with　Fe2+:SDS　(mol)=10:1,　its　surface　area　is　82.0　m2·g-1,　BJH　average　diameter　is　12.5　nm,　pore　volume　is　0.257　cm3·g-1,　and　the　mesoporous　ZnFe2O4　has　superstructure　of　stacking　strings　of　bead.