Based on a low temperature route (sol-gel autocombustion) a nano-ferrite CoFe2O4and Li0.5Fe2.5O4 and different percentages of cobalt-ferrite are synthesized. The crystalline structure by XRD and dielectric properties with TEM micrographs are presented. The XRD (crystallite size and lattice parameter) are determined which affected by cobalt content. TEM micrographs show a nano-particles in the range of (8-20) nm which correlate with crystallite size. Dielectric properties (dielectric constant, loss tangent and dielectric loss factor) are decreased with frequency and cobalt content.