A new composite of polymers and nanoparticles was used to prepare heterogeneous cation exchange membranes, the blends of polycarbonate (PC) and acrylonitrile butadiene styrene (ABS) as binders, the cation exchange resin powder as functional group agents, and the NiFe2O4 nanoparticles as additive. The integration of nanomaterials showed synergistic effects when combined with this blend of materials. Nickel ferrite nanoparticles were synthesized using co-precipitation method and the nanoparticles were analyzed using Fourier-transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), Vibrating sample magnetometer (VSM) and Field emission scanning electron microscopy (FE-SEM). The effect of nanoparticles content on the physicochemical and electrochemical properties of homemade membranes has studied in sodium chloride ionic solutions. Ion exchange capacity, water content, membrane potential, transport number, permselectivity, flux, electrical resistance and oxidation stability were investigated for the homemade membranes. The results showed that all physicochemical and electrochemical properties of membranes have improved with increasing nickel ferrite nanoparticles up to 2 wt % in the casting solution. The evaluation of prepared membranes with commercial membranes showed that the optimized membrane had good properties compared to commercial membranes.