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Nanoparticles of Fe-Co alloys and their oxides with the particle size below 20 nm were prepared by chemical vapor condensation process. The pure Ar, Ar+1%O2, Ar+3%O2 and Ar+6%O2 were used as carrier gases, with iron carbonyl and cobalt carbonyl as the precursors. XRD patterns showed that Fe-Co metallic nanoparticles were synthesized by using pure Ar as carrier gas,and only metal oxides were obtained using Ar+(>3)%O2 as carrier gas. The HRTEM images and TG-DTA curves were used to study the core-shell structure of the different nanoparticles. The nanoparticles obtained in pure Ar consist of black core and light shell with thickness of 2~4 nm. However, in the particles obtained in Ar+6%O2, the oxides core with visible lattice fringes are surrounded by thin shell.

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