Zinc oxide (ZnO) based nanomaterials have been used in various gas sensors due to the wide band gap (3.37 eV), large exciton binding energy and high mobility of charge carriers of ZnO. In this work, nano-crystalline ZnO nanofiber mats were synthesized through combined sol-gel electrospinning techniques followed by calcination, in which poly(styrene-co-acrylonitrile) and zinc acetate were used as the binder and precursor, respectively. Average diameter of the ZnO nanofibers decreased from 400 to 60 nm, while their grain size and crystallinity were enhanced by increasing the calcination temperature. Morphology and structure of the ZnO nanofiber mats were characterized by high resolution transmission electron microscopy, scanning electron microscopy, Fourier transform infrared spectroscopy and X-ray diffraction. ZnO nanofiber mats were found to be superhydrophilic (contact angle was close to 0 degrees) by contact angle measurements. The sensitivity of these ZnO nanofibers in detecting gaseous ammonia was tested using an indigenous set up. Due to their high surface area and superhydrophility, these ZnO nanofiber mats were highly sensitive in sensing gaseous ammonia and the sensitivity of these mats increased as a function of their calcination temperatures. (C) 2014 Elsevier Inc. All rights reserved.