Iron-based MIL-53 crystals with uniform size were successfully synthesized using a microwave-assisted solvothermal method and characterized by XRD, FE-SEM and DRS. We also investigated the photocatalytic activity of MIL-53(Fe) for the decomposition of methylene blue using H2O2 as an electron acceptor. From XRD and SEM results, the fully crystallized MIL-53(Fe) materials were obtained regardless of preparation method. From DRS results, MIL-53(Fe) samples prepared using microwave-assisted process displayed the absorption spectrum up to the visible region and then they showed the high photocatalytic activity under visible light irradiation. The MIL-53(Fe) catalyst prepared by two times microwave irradiation showed the highest activity.