Fe/Fe 3 O 4 nano-cubes and nano-octahedrons have been successfully synthesized by employing a facile solvothermal method at 180°C in the presence of ethylene glycol (EG). Well-defined assembly of uniform Fe/Fe 3 O 4 with an average size of 400 nm could be obtained without a size-selection process. X-ray diffraction, X-ray photoelectron spectroscopy, scanning electron microscopy and transmission electron microscopy were used to characterize the structure and morphology of the products. The magnetic properties of Fe/Fe 3 O 4 nanocomposite were measured by using a vibrating sample magnetometer. The result of magnetic characterization reveals that the magnetic polyhedrons exhibit a ferromagnetic behavior and possess high saturation magnetization. It is expected that these magnetic polyhedron with uniform size would have potential applications in recording media and electrode materials.