Fe60Co40 and Fe72Al28 nano-alloys were synthesized from elemental powders via highenergy mechanical alloying. The prepared samples were characterized using X-ray diffraction, scanning electron microscopy and X-band waveguide to measure the reflection loss in a frequency range of 9-10 GHz. The XRD patterns show that disordered Fe60Co40 solid solution with a bodycentred cubic structure is formed for milling times longer than 12 h, and after 4h milling, the solid solution Fe72Al28 has been largely formed. Morphological studies indicate an average grain size of 10 to 15 nm. The microwave- absorbing characteristic reveal good performance for Fe60Co40 compared to Fe72Al28, the maximum reflection loss is about -12 dB for the absorber.