The present work dealt with the preparation of carbon fibers from Polyacrylonitrile (PAN)/ acrylamide (AM) fibers via a solvent-free coagulation process. The PAN/AM fibers were stabilized in an oxidizing atmosphere at various temperatures (200, 250, 275, and 300 °C), while the stabilization time was fixed at thirty minutes. The effects of stabilization temperature on the chemical and the physical properties of the prepared stabilized fibers were studied. The chemical structure evolutions of stabilized fibers (SFs) from the precursor fiber were observed with FTIR studies, whereas the microstructure properties were thoroughly characterized with SEM studies. The mechanical strengths of the SFs were obtained from the Young Modulus and the tensile strength analyses. Stabilization temperature at 275°C had been identified as the optimum stabilization temperature for the PAN/AM fibers.