Nanocrystalline mixed lithium–chromium ferrites were prepared by using sol–gel method. The samples were sintered at different temperatures in air. Their structural and magnetic properties were studied by X-ray diffraction, scanning electron microscopy, transmission electron microscopy, Raman scattering, FT-IR and magnetic hysteresis loop tracer techniques. The X-ray diffraction patterns reveal that all the samples consist of nanocrystalline single cubic phase structure. The morphological studies of synthesized nanocrystalline samples were obtained from the scanning electron microscopy and transmission electron microscopy techniques. Raman scattering and FT-IR studies indicate that the spinel phase formation takes place at higher sintering temperature. The magnetic studies show that, the ferrimagnetic behavior increases with sintering temperature.