Extensive utilization of synthetic dyes in various industries poses a great threat to the environment. These dyes are toxic in nature and cause serious health problems in the living beings. The presence of these dyes in water also affects the photosynthetic activity of aquatic plants as they interfere with the incoming sun rays and gas dissolution. Although different methodologies have been adopted to treat the dye contaminated water but still many improvements have to be done. Metal oxide nanofibers present a better alternative in waste water treatment which are able to degrade the organic dyes using advanced oxidation processes. Herein, we have fabricated nickel oxide nanofibers using cost effective electrospinning technique with excellent photocatalytic activity in the presence of visible light to completely mineralize the highly recalcitrant diazo congo red dye. Development of such nanofibers for the degradation of highly stable dyes may act as a major component of nano-remediation processes in the near future.