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NiFe 2 O 4 /MWCNTs nanohybrids were synthesized via novel one step ultrasonication assisted method using ortho-xylene as a dispersive medium with varying MWCNTs concentration (0.0%, 1.0%, 1.5%, 2.0% and 2.5%). The nanohybrids were characterized by X-Ray Diffraction (XRD), Scanning Electron Microscope (SEM), Fourier Transform Infrared Spectroscopy (FT-IR) and Impedance Analyzer techniques. XRD indexed patterns confirmed the formation of NiFe 2 O 4 /MWCNTs nanohybrid. The SEM images showed the decoration of nickel ferrite nanoparticles on MWCNTs. The FTIR results show two absorption bands. The Cole-Cole plots of impedance show the resistance was only due to the grain boundary contribution. The dielectric properties were found to be increasing with increasing MWCNTs concentration. For 2.5% MWCNTs concentration, dielectric constant and loss 1.06×10 5 , 1.99×10 6 were achieved as compared to pure nickel ferrite 6.17×10 3 , 3.87×10 4 , respectively. Such increase in the dielectric properties renders its application at high frequency [ABSTRACT FROM AUTHOR]