Electrospun nanofibers of poly (vinyl alcohol) (PVA)/Lanthanum (III) chloride (LaCl(3)) composite were employed to prepare the LaOCl nanofibers by calcination. TG-DSC was used to investigate the thermal property of precursor, while FT-IR, XRD, FFSEM and TPD were employed to characterize the derived LaOCl nanofibers. Results indicate that the addition of LaCl3 leads to the formation of fork segments in the structure of electrospun PVA/LaCl(3) composite nanofibers, therefore, changing the decomposition behavior of the fibers. Pure LaOCl fibers with a diameter range of 90-220 nm can be obtained by calcination of electrospun PVA/LaCl(3) composite nanofibers at 700 degrees C for 7 h. The resultant LaOCl nanofibers show a good sensing behavior for CO(2) gas. (C) 2009 Elsevier B.V. All rights reserved.