A novel technique for the production of thiol-ene microspheres using acoustic resonance and coaxial flow is reported. The method utilizes low-frequency acoustically driven mechanical perturbations to disrupt the flow of a thiol-ene liquid jet, resulting in small thiol-ene droplets that are photochemically polymerized to yield thiol-ene microspheres. Tuning of the frequency, amplitude, and monomer solution viscosity are critical parameters impacting the diameter of the microspheres produced. Characterization by optical microscopy, scanning electron microscopy, and dynamic light scattering reveal microspheres of diameters <10 mu m, with narrow particle distributions. (C) 2016 Elsevier Ltd. All rights reserved.