The thermal oxidative stabilization and carbonization processes of poly(hexamethylene adipamide) or (polyamide 66) fibers were accomplished to transform into carbon fibers. Polyamide 66 fibers were pretreated with a ethanol solution of cupric chloride followed by a stabilization process in the air atmosphere. Carbonization experiments were executed at temperatures of 500, 700, 900, and 1100°C utilizing heating rate of 2.5 °C/min. Carbonization experiments were performed at temperatures between 500 and 1100°C employing the rises of 100°C. X-ray diffraction analysis of the carbon fibers shown a highly disordered carbon structure developed during the carbonization process. The values of fiber diameter, linear density, volume density, carbon fiber yield, elemental analysis, and electrical properties revealed a strong dependence on the carbonization temperature. As an insulating material, the polyamide 66 or PA66 precursor was transformed to a semiconducting stage after the thermal stabilization and carbonization processes. The current study demonstrated how processing parameters influence the structure and characteristics of carbon fibers produced from poly(hexamethylene adipamide) fibers.