We have successfully prepared Carbon/Fe-Co alloy composites starting from metal organic precursors synthesized by polymerized complex method. The carbon/Fe-Co alloy composites were obtained after the carbonization of the precursors heat-treated at ambient pressure and lower temperatures ranging from 500 to 700°C in N 2 gas flow. Crystalline sizes of both carbon matrix and Fe-Co alloy particles were determined by X-ray diffraction measurements as a function of the Co concentration and the carbonized temperature. The alloy particles were widely dispersed in the carbon matrix and the particle size carbonized at 600°C was about 20-50nm observed by scanning electron microscopy. The composite carbonized at 600°C had very small coercivity of 14 Oe and exhibited relatively large permeability spectra at frequency of GHz range.