Sb2O3 fibrils and tubules with lengths of up to several millimeters and diameters of nanometers to submicrometers were achieved by using Sb2S3 nanopowders as starting material. The synthesis can be ascribed to a vapor-solid process where metal catalyst was neither adopted during the synthesis, nor observed at tips of fibrils or tubules. Sb2O3 fibrils and tubules with lateral dimensions in nano- or submicron-scale may show enhanced catalytic and flame retardant performances. (C) 2002 Elsevier Science B.V. All rights reserved.