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FeSiAl alloys ribbons synthesized by melt-quench were annealed in vacuum at 873 K for 60 min. The flaky powders were prepared by milling the annealed ribbons for 70 h. After milling, the powders were heat treated at 573 K for 90 min. The ordering degree of the powders lattice structure was analyzed by X-ray diffraction (XRD).The measurement of specific saturation magnetization was carried out by vibrating samples magnetometer (VSM). Complex permittivity and complex permeability in the frequency band of 0.5-18 GHz were measured with the vector network analyzer. The ordering degree of the superlattice structure increased from 0.27 to 0.49. Complex permittivity and complex permeability decreased with increasing Si content. After ordering, the specific saturation magnetization decreased from 134.2 to 85.0 A.m2.kg-1.For use in anti-EMI material, the total contents of Si and Al in FeSiAl alloys should be controlled at a low level.