In this work, different synthesis routes from the anode and cathode of a spent nickel metal hydride (Ni-MH) battery were studied for the purpose of producing different ceramic precursors for the formation of nickel titanate (NiTiO 3 ). The precursors were subjected to heat treatments at different temperatures to form NiTiO 3 , in which samples 1A and 2A were obtained from the anode and sample 1C from the cathode. The metal content of the Ni-MH battery's active devices was determined by inductively coupled plasma optical-emission spectrometry. The contents were characterized by thermogravimetry, Fourier-transform infrared spectroscopy, Raman spectroscopy, scanning electron microscopy with energy-dispersive X-ray spectroscopy, transmission electron microscopy, and X-ray diffraction. The FTIR spectra of samples 1A, 2A, and 1C heat-treated at 800 °C with a 2 h isotherm indicated the existence of two main absorption regions in all the samples: the first, at 525 cm −1 , was attributed to Ti−O stretching, and the second, at 440 cm −1 , to the Ti−O−Ni bond attributed to the formation of NiTiO 3 . The Raman spectra of all of the samples obtained through the heat treatment showed intense vibrational modes for NiTiO 3 . The diffractograms occurrence of NiTiO 3 and TiO 2 phases was identified in all samples, which is in agreement with the data files PDF #33−0960 (NiTiO3, nickel titanate) and PDF #21−1276 (TiO 2 , rutile), it is important to highlight that the bunsenite phase, according to PDF #47−1049 (NiO), was observed in samples 1A and 1C. All the synthesis routes were successful in forming NiTiO 3 from the active material of the Ni-MH battery.