Niobophosphate glasses [(xNb2O5(0.5 − x)P2O5)0.5Li2O]: yFe2O3 were prepared by the melt-quenching method and analysed by means of infrared spectroscopy and x-ray powder diffraction. LiNbO3 crystals were detected for high niobium contents samples. The use of both techniques gives new information about the structure of niobium-phosphate glasses and glass-ceramics.