Zirconium nitride (ZrN) fibers were synthesized by carbothermal reduction and nitridation of composite fibers obtained by electrospinning. The structure and morphology of ZrN fibers were characterized by the scanning electron microscopy (SEM) and transmission electron microscopy (TEM). After calcinations at 1600 degrees C, the surface of ZrN fibers with average diameter about 500 nm is rough but the continuous microstructure was still maintained by the connection of irregular fine particles. The diameter of ZrN crystalline was in the range of 100-500 nm. Both X-ray diffraction (XRD) and Raman spectroscopy analysis indicated that the zirconium nitride fibers have a NaCl-structure cubic cell and the better crystallinity of grains. (C) 2008 Elsevier B.V. All rights reserved.