Industrial dye waste is highly toxic, nonbiodegradable, and has a significant negative impact on the environment. Photodegradation of phenothiazine derivative dyes by undoped Fe 3 O 4 nanoparticles (Fe 3 O 4 ), reduced graphene oxide (rGO)-doped Fe 3 O 4 nanocomposites (G@Fe 3 O 4 ), nickel-doped Fe 3 O 4 nanoparticles (Ni@Fe 3 O 4 ), and graphene-nickel codoped Fe 3 O 4 nanocomposites (Ni/G@Fe 3 O 4 ) is achieved using a facile coprecipitation technique. The X-ray powder diffraction patterns of all the prepared samples confirm the face-centered cubic structure of metallic Fe 3 O 4 . The crystallite size of the Ni-doped samples increases, indicating that the addition of Ni 2þ significantly increases the crystalline grain growth of Fe 3 O 4 , whereas the addition of graphene dopants results in a decrease in the particle size and an increase in the bandgap. The higher specific surface area of Ni/G@Fe 3 O 4 (70.082 m 2 g À1 ) is attributed to the introduction of rGO nanoflakes and the formation of secondary pores. The X-ray photoelectron spectra of O 1s, C 1s, Ni 2p, and Fe 2p confirm the presence of oxygen anions, graphene, Ni 2þ ions, and Fe 3þ and Fe 2þ oxidation states in the Fe 3 O 4 lattice.