Nitriding of surface of aluminum alloys was carried out with using an electron-beam-excited-plasma (EBEP)technique. The EBEP is sustained by electron impact ionization with energetic electron beam. Two kinds of substrates,aluminum alloys AA5052 and AA5083, were exposed to the down flow of EBEP source at 843 K for 45min. The specimens were characterized with respect to following properties: crystallographic structure (XRD), morphology (SEM) and the cross sectional microstructures of the nitrided layer was observed using a scanning electron microscopy (SEM). There are some Al2O3 particles on the surface of the nitrided AA5052 and AA5083. The AIN layers were formed on the substrates with the thickness of 4.5 μ m for AA5052 and 0.5 μ m for AA5083. A relatively uniform nitrided surface layer composed of AIN can be observed on the AA5052 substrate. The grains size near the interfaces between the substrate and AIN layer were smaller than that near the surface. On the surface of AIN layer, the concentration of nitrogen was high and in the middle of AIN layer it had a constant concentration like the aluminum and the concentration was decreased with approaching to the interface. On the surface of nitrided AA5083, a uniform AIN layer was not formed as the reason for the high nitriding temperature.