Pure and mixed ZnO-SiO2 particles were made by flame-spray pyrolysis of zinc acetate and hexamethyldisiloxane or SiO2 sol dispersed in methanol or water-in-oil emulsion, respectively. The product particles were characterized by nitrogen adsorption, infrared absorption, and X-ray diffraction. The evolution of solid or hollow particle formation along the flame axis was unraveled by transmission electron microscopy after collection by thermophoretic sampling. The effects of silicon precursor and solvent on product particle characteristics were evaluated. The characteristics of the product particles were controlled by the Si precursor and solvent.