In the present study, electrospun PAN precursor webs and the stabilized and carbonized nanofiber webs processed under different heat-treatment conditions were characterized by means of weight loss measurement, elemental analysis, scanning electron microscopy (SEM), attenuated total reflection-Fourier transform infrared spectroscopy (ATR-FTIR), differential scanning calorimetry (DSC), thermogravimentric analysis (TGA), and X-ray diffraction (XRD) analysis. The result indicated that stabilization and carbonization processes with different temperatures and heating rates significantly influenced the chemical and morphological characteristics as well as the thermal properties of the stabilized and then subsequently carbonized nanofiber webs from PAN precursor webs. It was noted that the filament diameter and the carbon content of a carbonized nanofiber web as well as its weight change may be effectively monitored by controlling both stabilization and carbonization processes.