Continuous NiTiO3 nanofibers have been successfully synthesized by a sol-gel assisted electrospinning method followed by calcination at 600 A degrees C in air. These nanofibers were characterized for the morphological, structural and optical properties by scanning electron microscopy (SEM), energy-dispersive X-ray spectrum (EDS), transmission electron microscopy (TEM), X-ray diffraction (XRD), X-ray photoelectron spectra (XPS) and UV-visible (UV-vis) diffuse reflectance spectroscopy (DRS). SEM results reveal that the obtained NiTiO3 nanofibers are 175 nm in diameter and several micrometers in length after annealing at 600 A degrees C. The XRD analysis shows that the nanofibers possess highly crystalline structure with no impurity phase. In contrast, the NiTiO3 nanoparticles synthesized at the identical conditions by a sol-gel route have impurities including TiO2 and NiO. Moreover, the electrospun NiTiO3 nanofibers are endowed with an obvious optical absorbance in the visible range, demonstrating they have visible light photoresponse.