Manganese-Zinc Ferrite is a very high permeability magnetic material. The permeability is depended on the amount of manganese and zinc used in the synthesis of ferrite material.Reagent graded raw materials were used as initial material to synthesize and get a characterization of Mn-Zn based spinel ferrite. The nanocrystalline powders of manganese ferrite were obtained by the process of citrate precursor method. The obtained nanocrystals of Mn-Zn were doped by Gadolinium which further it was employed to produce specimens of Mn0.5Zn0.5GdxFe2-xO4 (x = 0, 0.01, 0.03). The study of doped (Gd) Mn-Zn ferrite nanocrystals was characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM). The results of XRD data determine the average crystallite size of doped (GD) Mn-Zn nanocrystals in the range of 40nm to 45nm. The images obtained through FE-SEM shows the flake-like structure of doped (Gd) Mn-Zn ferrite nanocrystals. Further studies of doped (Gd) Mn-Zn ferrite were done by FTIR and Raman spectroscopy.