In situ TEM oxidation study of Fe thin-film transformation to single-crystal magnetite nanoparticles

In this work, we present an in situ transmission electron microscopy (TEM) study of Fe thin films to Fe nanoparticle formation and their oxidation to single-crystal magnetite nanoparticles. Amorphous Fe thin films were prepared by sputtering on TEM carbon grids. The thin Fe films were continuously heated in situ from room temperature to 700 °C under vacuum (4 × 10–4 Pa). With the increase in temperature, the continuity of the thin film starts breaking, and Fe nanoparticle nucleation centers are formed. At 600 °C, the thin film transforms into metallic Fe nanoparticles (NPs) with a small presence of different Fe oxide NPs. Further increase in the temperature to 700 °C resulted in the full oxidation of the NPs (i.e., no core–shell were found). Zero-loss energy filtered diffraction and HRTEM analysis of the lattice spacing reveals that all NPs have fully transformed into single-phase magnetite NPs. The structural study of the magnetite NPs shows that magnetite NPs are free of antiphase domain boundary defects. This work demonstrates that under low partial pressure of oxygen at elevated temperatures a complete oxidation of Fe NPs into magnetite single-crystal nanoparticles can be achieved.