New techniques are used to synthesis and characterize 0.5BaTiO3/0.5Ni0.5Zn0.5Fe2O4; (BTO/NZF) multiferroic nanocomposite. Improved citrate autocombustion preparation technique is used to synthesis ferromagnetic and ferroelectric phases of the investigated nanocomposite. Atomic force microscope (AFM) is one of the important tools for imaging, measuring, and manipulating matter at the nanoscale. AFM is used at different sample areas to confirm the data obtained from scanning electron microscope (SEM) and transmission electron microscope (TEM). Moreover AFM gives 3D visualization for the surface texture and roughness showing the morphology of the two distinguishes phases. The traditional characterizations techniques have been used such as X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR) to identify the formation of the two individual phases separately and to study the chemical composition of the prepared nanocomposite respectively.