Aerosolization of polystyrene solutions followed by drying in a tubular furnace produced submicron-sized polystyrene particles. Characterization using x-ray diffraction, scanning electron microscopy (SEM), and infrared spectroscopy (FT-IR) revealed that the particles were amorphous, spherical, and free of residual solvent. The average particle size and size distribution varied with furnace temperature, the initial polystyrene solution concentration, and solvent type. The particles’ BET-based specific surface area depended upon these parameters as well as the carrier gas flow rate. Analysis of the competing rates of convection, solvent evaporation, droplet collisions, and polymer diffusion help to rationalize the results. The dependence of the solvent evaporation rate on temperature controls the particle diameter, but droplet coalescence cannot be ignored. Long residence times and high furnace temperatures softened the particles; after filtration, polymer diffusion between solid particles produced visual evidence of partial coalescence.