AbstractSpherical, highly porous synthetic carbon particles have been prepared from formulations of either poly(furfuryl alcohol) or poly(vinyl acetate) mixed with a solvent and poreforming agents. Production was carried out by atomizing these mixtures inside a thermal reactor and drying the resulting aerosol. The size of the collected polymeric particles was controlled by preadjusting the parameters of the atomization process. Fine‐tuning of the process resulted in the generation of batches of monosized particles. Subsequent thermal degradation at 600°C resulted in porous chars with controlled pore‐size distributions. Several distinct pore structures were superimposed using this technique with pore widths spanning the region from a few nanometers to a few tens of micrometers. Spherical and equal‐sized macropores were also generated with a special technique described herein. All chars were produced in batches of spherical and monodisperse particles, with diameters in the range of 20–150 μm. BET surface areas were measured to vary from 1 m2/g to over 150 m2/g prior to any oxidative treatment. Porosities varied from
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