Phenolic/furfural (P/F) gel microspheres have been successfully produced by a new supercritical CO2-based process. CO2-soluble poly(dimethylsiloxane) (PDMS) was used as the stabilizer in this system. The spherical morphology of the gel microspheres was confirmed by scanning electron microscopy. The particle size and particle size distribution of the P/F gel microspheres can be modified upon variation of the solids content and the stabilizer content. The resultant P/F microspheres have an average particle size in the range of 1-6 mu m. The structure of the P/F gel microspheres was revealed by IR analysis. (C) 2000 Elsevier Science B.V. All rights reserved.