In this work, pure and Ni-doped SnO 2 hollow nanofibers with porous structures were fabricated through combination of electrospinning technique and calcination procedure. The hollow SnO 2 nanofibers were characterized by means of scanning electron microscopy (SEM), transmission electron microscopy (TEM), thermogravimetric analyzer (TGA), X-ray photoelectron spectroscopy (XPS) and their gas sensing properties for acetone were also investigated. A high heating rate in calcination process would lead to the formation of hollow SnO 2 nanofibers with a tube-like structure. Hollow Ni-doped SnO 2 nanofibers could be prepared by adjusting Ni 2+ concentration in the precursor solution using a facile process with appropriate thermal treatment. Comparative gas sensing properties revealed that Ni-doped SnO 2 hollow nanofibers exhibited a much higher response in detecting acetone vapor than both pure SnO 2 hollow nanofibers and Ni-doped SnO 2 solid nanofibers at the same temperature. The excellent sensing performances of Ni-doped SnO 2 hollow nanofibers were ascribed to its hollow-core structure and Ni doping.