In the present work, nanocrystalline Sb 3+ ions doped Ni0.2Ba0.1Co0.7Fe2-xSbxO4 (0≦x≦0.1, step by 0.025) ferrites were prepared via sol-gel method. The spinel-phase structure of samples can be confirmed by X-ray diffraction (XRD) patterns. The composition and structure were further studied by fourier transform infrared spectroscopy (FTIR). There were two typical characteristic bands 1 and 2 related to the stretching vibrations in spinel ferrite in FTIR spectra. Energy dispersive spectrometer (EDS) analyzed the elements of samples. It indicated that the elements of Ni, Ba, Co, Fe, O and Sb existed in the samples. Vibrating sample magnetometer was used to characterize magnetic properties. The saturation magnetization decreased from 57.65 emu/g to 44.50 emu/g with the increasing Sb 3+ions content, which is attributed to Fe 3+ ions replaced by the Sb 3+ ions. Remanent magnetization and coercivity first decreased and then increased slightly.