Petr Synek, Ondřej Jašek, Lenka Zajíčková
Study of Microwave Torch Plasmachemical Synthesis of Iron Oxide Nanoparticles Focused on the Analysis of Phase Composition
Plasma Chem. Plasma Process. 34 (2014) 327-341
This work presents the results obtained on the single-step route towards the synthesis of iron oxide nanoparticles in a microwave plasma torch. The torch is supplied by 660 sccm of Ar mixed with 1 sccm of Fe(CO)(5) and a variable amount of O-2. The influence of oxygen addition on the phase composition of the synthesized powder was studied. Magnetite and maghemite phases could not be distinguished using the standard X-ray diffraction (XRD) analysis. Therefore, a combined XRD and Raman spectra analysis had to be applied, which is based on fitting of selected diffraction peaks and spectral features. According to XRD and Raman spectroscopy, the powder synthesized from Ar/Fe(CO)(5) consisted about 50 % of magnetite, Fe3O4, the rest being alpha-Fe and FeO. An increase in oxygen flow rate led to an increase in gamma-Fe2O3 percentage, at the expense of alpha-Fe, FeO and Fe3O4. Almost pure gamma-Fe2O3 was synthesized at oxygen flow rates 25-75x higher than the flow rate of Fe(CO)(5). A further increase in the oxygen flow rate led to alpha-Fe2O3 and epsilon-Fe2O3 production. The distributions of nanoparticles' (NPs) diameters were obtained using transmission electron microscopy (TEM) and dynamic light scattering (DLS). The mean diameter of the NPs measured by TEM was 13 nm while the DLS measurements led to the mean diameter of 12 nm. About 90 % of all particles had the diameter in the range of 5-21 nm but a few larger particles were observed in TEM micrographs.
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