Ultrafine spherical maltodextrin and maltose particles were successfully produced with the antisolvent vapour precipitation (AVP) technique. Comparison between the two materials confirmed that a key requirement for the process is in inhibiting crystallization of the material. The precipitation process consists of: (1) an initial phase separation forming an emulsion formation, (2) phase inversion and (3) finally a water-maltodextrin shrinkage phase which forms the spherical particles driven by interfacial surface tension. Dehydrating the droplet at different stages of the process resulted in various particle morphologies; porous, smooth, microsphere network and microspheres. Higher ethanol relative humidity, higher ethanol absolute humidity and lower initial weight concentration were found to favour the formation of amorphous microspherical particles upon drying. (C) 2015 Elsevier B.V. All rights reserved.