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We studied the effect of the mixed phase of nickel oxide–gallium oxide–graphene (NiO-Ga₂O₂/G) heterostructure nanocomposite on the photocatalytic degradation of Congo red dye. The effect was investigated based on NiO-Ga₂O₂ junction, NiO-graphene, and Ga₂O₂-graphene contacts. The laser-induced graphene was embedded into NiO and NiO-Ga₂O₂. Raman spectra confirmed the fabrication of disordered graphene and the mixed phase between the oxides and graphene. HRTEM showed that very fine nanoparticles for both NiO and Ga₂O₂ with a size of ~7–10 nm were synthesized. Elemental compositional expressed the formation mixed phase. The effect of graphene content was investigated at 2 and 10% wt with NiO and the heterojunction of NiO-Ga₂O₂. The photocurrent studies was measured of these nanocomposite film deposited on two interdigitated gold electrodes, biased by 5.0 V and irradiated by the UV source. The results of photocatalysis measurements indicated an improvement occurred upon the heterojunction between Ga₂O₂ and NiO, however, a dramatic improvement was observed with the addition of graphene of 10%. The results expressed that the ternary phase of p-NiO/n-Ga₂O₂/graphene is promising in the photocatalytic application toward Congo red decomposition.