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The formation of mixed metastable phases as a result of ion‐beam mixing of the Al‐Fe‐Mn system with 100‐keV Ar+ ions and their subsequent transformations upon thermal annealing have been studied. The mixed state is comprised of both binary (Fe‐Al, Fe‐Mn, Mn‐Al) and ternary (Al‐Fe‐Mn) metastable phases. Conversion‐electron Mössbauer spectroscopy and low‐angle x‐ray diffraction studies reveal the formation of disordered phases upon ion beam mixing, which acts as a precursor for the growth of the equilibrium phases upon thermal annealing via lowering of kinetic barrier for the reactions.