Ferrites are a large class of oxides with remarkable magnetic properties. Their applications include an impressive range extending from millimeter wave integrated circuitry to power handling, simple permanent magnets, and magnetic recording. These applications are established upon the very basic properties of ferrites such as saturation magnetization, high electrical resistivity, low electrical losses, and a very good chemical stability.In the present study aSeries of Cobalt substituted Calcium Hexaferrite samples with composition CaFe12-xCoxO19 (0 ≤ x ≤ 4), have been prepared by Solution combustion synthesis. The structural properties and morphology of the samples were studied with XRD, and SEM. Electrical properties were studied with the help of LCR meter. The XRD studies of all samples confirmed the formation of single-phase M-type hexagonal ferrites with the space group of P63/mmc. Grain size, lattice parameters and volume of the samples are calculated. Volume of the cell is found to decrease with increase in the Cobaltsubstitution. The SEM analysis revealed that the particles are of uniform grain morphology and Nano in size. Frequency dependency of dielectric properties, frequency and temperature dependency of Electrical properties are studied. Resistivity at room temperature, Activation energy and transition temperature are reported.