Iron nanoparticles were prepared by selective leaching method. Initially the rapidly solidified AlFe11 alloy was prepared and consequently the aluminium matrix was dissolved from this alloy in 20% NaOH solution. This process was carried out at 0 and 80°C. At lower temperature, the iron nanoparticles covered by thin layer of Fe(OH)₃ were successfully obtained. The size of formed nanoparticles was about 8 nm and the particles exhibited massive agglomeration. It is not limitation of the process, because the application of nanoparticles is as a precursor for production of bulk nanocrystalline materials (metals, alloys and metal matrix composites). At higher temperature, the selective leaching process failed and iron was oxidized to different hydroxides. Aluminium containing waste liquid from selective leaching was used for production of powder Al₂O₃. Initial alloys and products were characterized by X-ray diffraction, scanning electron microscopy, and high resolution transmission electron microscopy.
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