This work presents the investigation, at room temperature, of Zn 2 TiO 4 samples containing Ni 2+ ions as substitutional impurities. Samples with molecular formula Zn 2(1-x) Ni 2x TiO 4 , where x = 0.00, 0.0007, 0.001, 0.0013, 0.002 and 0.003, in which Zn 2+ ions were replaced by Ni 2+ ions, were prepared through solid-state method, crystalline data were obtained by X-ray diffraction, the elemental composition was determined by X-ray fluorescence and the optical properties were investigated through photoluminescence and photoacoustic techniques. The photoluminescence spectra showed broadbands from 640 nm to 800 nm. The emission of the Zn 2(1-x) Ni 2x TiO 4 samples was assigned to the overlapping of the Ni 2+ and the Zn 2 TiO 4 emission. The most intense photoluminescence signal was obtained with excitation radiation at a wavelength of 360 nm for the sample with x = 0.001. The photoacoustic spectra showed absorption bands characteristic of semiconductor materials due to the host Zn 2 TiO 4 . The energy bandgap of the Zn 2(1-x) Ni 2x TiO 4 was obtained from photoacoustic absorption spectra.