Microwave Assisted Synthesis of Iron(III) Oxyhydroxides/Oxides Characterized Using Transmission Electron Microscopy, X-ray Diffraction, and X-ray Absorption Spectroscopy.

Microwave assisted synthesis of iron oxide/oxyhydroxide nanophases was conducted using iron(III) chloride titrated with sodium hydroxide at seven different temperatures from 100 degrees C to 250 degrees C with pulsed microwaves. From the XRD results, it was determined that there were two different phases synthesized during the reactions which were temperature dependent. At the lower temperatures, 100 degrees C and 125 degrees C, it was determined that an iron oxyhydroxide chloride was synthesized. Whereas, at higher temperatures, at 150 degrees C and above, iron(III) oxide was synthesized. From the XRD, we also determined the FWHM and the average size of the nanoparticles using the Scherrer equation. The average size of the nanoparticles synthesized using the experimental conditions were 17, 21, 12, 22, 26, 33, 28 nm, respectively for the reactions from 100 degrees C to 250 degrees C. The particles also had low anisotropy indicating spherical nanoparticles, which was later confirmed using TEM. Finally, XAS studies show that the iron present in the nanophase was present as iron(III) coordinated to six oxygen atoms in the first coordination shell. The higher coordination shells also conform very closely to the ideal or bulk crystal structures.