Changes in structural and magnetic properties have been systematically induced in lithium niobate (LiNbO 3) powders, Fe-doped with different concentrations and thermally treated in oxidized and reduced states. A rather strong ferromagnetic response at room temperature with a saturation magnetization of 0.96 Am 2 kg −1 was obtained for the higher utilized doping concentration, which is of the order of 1% mol. This may be considered a first report of the manifestation of ferromagnetism in nanocrystalline lithium niobate powders within the regime of very low Fe-doping concentrations. Post-thermal treatment in a controlled atmosphere is key for inducing and detecting this behavior, which can also be explained as the effective recombination of Fe impurities with oxygen vacancies in the surface of the material. Mechanochemical-calcination was employed for the synthesis of LiNbO 3 powders and after that, a diffusion process of 0.44%, 0.89%, 1.47% and 2.20% mass of Fe 2 O 3 was used in the Fe-doping. Oxidation and reduction processes were performed using a controlled atmosphere of ultra-high purity oxygen and hydrogen, respectively. X-ray diffraction and Raman spectroscopy were employed to characterize the materials. The magnetic properties were studied using Vibration Sample magnetometry and Electron Spin Resonance spectroscopy.