The composites of Fe-Si-Al alloy flakes and dielectric polymer were mainly characterized by transmission and conversion electron Mossbauer spectrometry (TMS and CEMS). The Fe-Si-Al flakes were prepared by milling the Sendust powder (9.8mass%Si, 5.9mass%Al, and balance Fe) in n-hexane solvent for several hours and days. The deformed structures were estimated by magnetic hyperfine field distributions, and further the annealing effects were investigated. The composites of Fe-Si-Al alloy forged for less than 100 hours recovered high permeability with production of DO₃ structure after annealed at 650°C for 2 hours in Ar atmosphere. However, the polymer composites of Fe-Si-Al alloy flakes forged for 180 hours, which could apply to new noise suppression filter in several GHz frequency bands, gave broad hyperfine distributions with high magnetic fields. The forged flakes were decomposed into a-Fe in the bulk and Fe species dispersed in Si or Al interface beneath the Si and Al oxides surface by annealing.