New chemical synthesis procedure for the preparation of nickel zinc doped W-type hexagonal barium ferrite and aluminium doped yttrium-iron garnet nanoparticles has been developed, using the nitrate-citrate sol-gel auto-combustion method (NCSAM). The crystalline phase attributes, microstructure, morphology, specific surface area, Curie temperature (TC), permeability, thermal behavior of the as-burnt phase and the heat treated powders were characterized using XRD, SEM, FT-IR, BET, TG-DTA and AC magnetic permeability with frequency shift. In the case of the hexaferrite, the pure W-type ferrite phase is formed during 4 hour annealing at a temperature of 1200 °C, the garnet phase is formed at a lower temperature i.e. 1000 °C. Furthermore it has been confirmed, that the AC magnetic permeabilities of the garnet materials are strongly depending on the chemical composition.