Nanocrystalline Ti-substituted zinc ferrite was synthesized by sol–gel autocombustion route. Structural characterization of the sample was carried out by the X-ray diffraction technique which confirms that it is a single phase cubic ferrite. The FTIR spectra revealed two absorption bands which are attributed to the fundamental vibrational modes of tetrahedral and octahedral complexes of the unit cell. The IR bands due to tetrahedral complexes are found to shift slightly towards higher frequency side where as that due to octahedral complexes are found to shift towards lower frequency side. The particle size of the Ti-substituted zinc ferrite was estimated to be ∼30 nm. The elemental analysis as obtained from EDAX is in close agreement with the starting composition used for the synthesis. Vibrating sample magnetometer (VSM) studies indicated that this sample is ferrimagnetic in nature at room temperature.