New method for preparation of Fe3O4 thin films using annealing Fe2O3 and Fe multilayer in vacuum is investigated in this work. Primal structures for annealing (Fe2O3 and Fe) were formed by reactive magnetron deposition method, using special construction facing target sputtering system with Fe planar targets. Crystal structure of as deposited thin film system, structural changes of this system after annealing at different conditions and phase composition formation were measured and analyzed using XRD method. The surface morphology was investigated by AFM (Atomic Force Microscopy). Samples magnetic properties were measured with MFM (Magnetic Force Microscopy) and magnetization curves measuring. The results show that it is possible to synthesize magnetite thin film using this method. A size of crystallites depends on synthesis condition. (c) 2005 Elsevier B.V. All rights reserved.