Cu-S-codoped TiO2 NPs supported on carbon nanofibers were prepared by the simple electrospinning method followed by calcinations at 800 degrees C in an argon atmosphere. The nanocomposite was characterized by the standard techniques. Results indicated that the Cu-S-codoped TiO2 NPs was covered by the graphite layer. This layer revealed an excellent adsorption behavior. Moreover, this layer has good electrical properties that can enhance electron transfer during the photocatalytic process. The Cu and S can decrease the band gap that suppresses the electron-hole recombination process. It subsequently enhanced the photocatalytic activity. The prepared nanocomposite appeared to have better adsorption and photocatalytic behavior than that of TiO2 CNFs for decolorization of reactive black 5 (RB5). Kinetic study indicated that adsorption and photocatalytic processes are closed to a pseudo first order model.