Synthesis mechanism, phase transfer and optical tracking of iron oxide nanoparticles
Colvin, Vicki L.
Doctor of Philosophy
High temperature synthesis of nanocrystals in non-polar solvents typically produces materials with narrow size distribution and high yields. However, the mechanism leading to the preservation of monodispersity on depletion of monomers is not understood, for example, in the case of iron oxide nanoparticles. In our study, it was found that oleic acid, a surfactant added to the mixture of iron precursor and solvent, gradually decomposed to release carbon monoxide at 320°C. This strong reducing gaseous product had a substantial impact on the size distribution of nanocrystals produced. The reduced forms of iron oxide catalyzed the disproportionation of carbon monoxide resulting in a graphitic carbon deposit on the surface of nanoparticles. The graphite coating inhibited further growth of particles and prevented Ostwald ripening. Graphite presence was demonstrated by Raman spectroscopy and Fourier transform infrared spectroscopy. It was found that the amount of graphite deposited on the surface of nanocrystals increased with time at 320°C. Quantitative data regarding the carbon content was obtained by thermo gravimetric analysis and energy dispersive spectrometry. The surface activity of the nanocrystals was shown to be affected by the carbon coating in applications such as arsenic removal.