In this study, a novel and simple approach to fabricate zirconium dioxide (ZrO 2) nanofibers by critical bubble electrospinning and subsequent thermal treatment was reported. The influences of different matrixes, weight percentages, heating rates, post-processing techniques, and with/without carbonization were discussed. The fiber size grew linearly with the increasing amounts of particles added. In addition, ZrOCl 2 /PAN composite fibers were converted to ZrO 2 nanofibers after high-temperature calcination, whose crystal structure was cubic phase of ZrO 2 after 1000 C, and the obtained ZrO 2 nanofibers shows excellent high-temperature-resistant adsorption and separation properties.