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Electron-Beam Physical Vapor Deposition of Iron Nanoparticles and their Thermal Stability in the Fe–O System

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Chemically pure (ligand-free) 5–70 nm iron nanoparticles were synthesized by electron-beam physical vapor deposition (EB-PVD) in a porous NaCl matrix. The influence of chemical composition, substrate temperature, and isothermal treatment on the dimensional, structural, and phase composition of nanoparticles in the Fe–O system was studied. For this purpose, independent molecular fluxes of Fe and NaCl were applied to a fixed substrate by electron-beam physical vapor deposition (EB-PVD) at substrate temperatures of 45–400°C to produce 3–30 wt.% Fe–NaCl condensates. With increasing iron content, substrate temperature, and heat treatment temperature, the average size of particles in the Fe–O system became greater. To study the oxidation kinetics of iron nanoparticles, the condensates produced at a substrate temperature of 45°C were isothermally treated in air at 200–650°C. The condensates were examined by scanning electron microscopy, transmission electron microscopy, and X-ray diffraction, and aqueous solutions of the condensates by dynamic light scattering. Being of small size and thus having high adsorption capacity for air and moisture oxygen, iron exothermally oxidized in the condensate when the vacuum chamber was opened and the condensate was separated from the substrate. At different substrate temperatures and after heat treatment, the nanoparticles may contain pure iron and iron oxides Fe3O4 and Fe2O3. In the studied condensates, the α-Fe phase is present only when the iron content is more than 20 at.%. This is explained by the fact that not all nanoparticles (crystallites) have time to oxidize to the Fe3O4 phase with increase in their sizes. In addition, Fe3O4 nanoparticles additionally adsorb oxygen. The ratio between the atomic percentage of oxygen and iron depends on the amount of iron, decreases with increasing iron content of the condensate, and even exceeds the value for the stoichiometric composition of Fe2O3, being equal to 1.5. The study shows that the EB-PVD method is universal in the use of inorganic materials for the synthesis and retention of pure nanoparticles of metals and their oxides.

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Acknowledgements

The effort was funded from the budget Ukrainian program “Support in the Development of Priority Research Areas” (KPKVK 6541230).

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Authors and Affiliations

  1. Paton Electric Welding Institute, National Academy of Sciences of Ukraine, Kyiv, Ukraine

    Yu.A. Kurapov, S.Ye. Lytvyn, G.G. Didikin & S.M. Romanenko

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  1. Yu.A. Kurapov
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  2. S.Ye. Lytvyn
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Correspondence to S.Ye. Lytvyn.

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Translated from Poroshkova Metallurgiya, Vol. 60, Nos. 7–8 (540), pp. 80–94, 2021.

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Kurapov, Y., Lytvyn, S., Didikin, G. et al. Electron-Beam Physical Vapor Deposition of Iron Nanoparticles and their Thermal Stability in the Fe–O System. Powder Metall Met Ceram 60, 451–463 (2021). https://doi.org/10.1007/s11106-021-00256-8

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