Incorporation of the transition metals nanoparticles can strongly modify the physiochemical characteristics of the metal oxides nanostructures. In the literature, preparing this interesting class of materials was achieved by sophisticated processes. In the present study, Ni(0)-doped TiO2/C nanofibers were successfully prepared by simple, effective, high yield and low cost technique; electrospinning. Calcination of electrospun nanofiber mats composed of titanium isopropoxide, poly(vinyl pyrrolidone) (PVP) and nickel acetate tetrahydrate in Ar/H-2 atmosphere at 700 degrees C led to produce good morphology Ni(0)-doped TiO2/C nanofibers. The introduced nanofibers revealed distinct performance as a photocatalyst for ammoniaborane hydrolysis due to the synergistic effect of the individual compounds as well as improving the photocatalytic performance of TiO2. Typically, after 30 min (at 25 degrees C), the obtained hydrogen equivalent was 2.1 and 1.1 for Ni(0)-doped TiO2/C and TiO2/C nanofibers, respectively. Moreover, the introduced nanofibers behave as an efficient photocatalyst to remove the methylene blue (MB) dye from water. Overall, the present study might open a new avenue to prepare the metal-doped metal oxide nanofibers using simple strategy. (C) 2012 Elsevier B.V. All rights reserved.