Y2O3 particles of various sizes have been prepared by flame spray pyrolysis using water-in-oil emulsion precursor solutions. We found that by varying the emulsion droplet size, the particle size of the prepared Y2O3 powder can easily be varied from 30 to 700 nm. In conventional spray pyrolysis, each droplet generated by the atomizer is converted to one particle. Thus, particle size can only be controlled by varying the concentration of the precursor, which results in a decrease in the generation rate. As in conventional spray pyrolysis, the flame spray pyrolysis of the emulsions was found to result in the conversion of one emulsion droplet to one particle. Control of particle size was achieved by varying the emulsion droplet size, which results in no decrease in the particle generation rate.