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Iron aluminide Fe₃Al nanostructures were synthesized by chemical reduction of iron(II) chloride via aluminum nanoparticles in the solid state. Aluminum nanoparticles (AlNPs) were prepared by a novel wire drawing method in the presence of lubricating oil. Chemical reduction of iron(II) salts in aqueous solution by metallic aluminum has a many mechanistic considerations. These mechanistic aspects were available by understanding the mechanism of electron transfer reactions between metal complexes. Here the mechanochemical reaction between aluminum nanoparticles and crystalline iron(II) chloride occurred by inner sphere electron transfer mechanism. The products were characterized by IR, UV–Vis, XRD, FESEM, and VSM. The weight fraction of iron aluminide nanoparticles calculated by the Rietveld method. Quantitative XRD analysis show a weight fraction of Fe₃Al 87% and unreacted metallic aluminum …