Indium oxide microspheres were synthesized for potential use in novel, polymer-based antistatic coatings for exposed spacecraft surfaces. Non-agglomerating indium oxide microspheres with diameters ranging from 0.5–2.0 μm were produced using an aerosol spray pyrolysis technique. The precursor solution used to generate the aerosol droplets for pyrolysis consisted of indium acetate dissolved in water; however, the actual indium species present in solution was identified as the hydrolysis product, dihydroxy(acetato)indium. Thermogravimetric analyses of commercial indium acetate and of pure crystals of the dihydroxy(acetato)indium compound both demonstrated clean solid-state pyrolyses to generate pure indium oxide, as confirmed by x-ray diffraction and infrared spectroscopic analysis. Air was used as the carrier gas for the aerosol droplets for the spray pyrolysis experiments, and pyrolysis took place within a 2′′ tube furnace. The microspheres were characterized by x-ray diffraction and scanning electron microscopy. The non-agglomerating characteristics of the microspheres, combined with their small size, indicates that these particles are highly promising for dispersion within a polymer matrixes required for novel polymer-based antistatic films.