A flame aerosol reactor was used to synthesize Fe(III)-doped titania powders. The processing conditions were controlled to obtain varying ratios of Fe:Ti in the as processed powders. The iron was incorporated into the titania lattice and promoted the conversion of the anatase to the rutile phase. With an increase in the iron dopant concentration, a decrease in the crystal size of the resultant titania particles was observed, along with a conversion to the amorphous state. The defect structure was further explored by Raman spectroscopy, revealing an increased shift and broadening of the anatase peaks with an increasing iron dopant concentration, and was attributed to shrinkage in the grain size. Absorption spectra revealed a shift of the absorption band toward the visible frequencies. Powders with Fe:Ti ratio exceeding 0.8 resulted in a binary mixture that had superparamagnetic characteristics.