The present study delves into the production of carbon nanofibers (CNFs) utilising electrospun polyacrylonitrile (PAN) nanofiber mats, with a specific focus on the influence of oxidative stabilisation and carbonisation treatments. This research aims to thoroughly understand how variations in stabilisation time and temperature, as well as carbonisation temperature, impact the CNFs properties. These properties include fiber size, morphology, chemical and crystal structure transformation, thermal behaviour, and surface characteristics. Our methodology involved a detailed examination of the thermal treatment processes, where we observed a significant decrease in fiber size, though the surface morphology of the fibers remained largely unaffected. We employed Fourier-transform infrared (FTIR) spectroscopy to track the transformation of nitrile groups in PAN to imine groups, which indicated the progression of cyclisation reactions. Complementary analyses through differential scanning calorimetry (DSC) confirmed a high degree of these reactions, particularly at stabilisation temperatures extending to 250 °C and beyond. The cyclisation process was found to be complete during the carbonisation phase, at temperatures reaching 450 °C and above. Further, x-ray diffraction (XRD) patterns offered insight into the changes in the crystal structure, particularly in the packing of the d(002) spacing because of the stabilisation and carbonisation processes. This findings from this study not only elucidate the intricate process of CNFs production from electrospun PAN nanofiber mats but also highlight the critical factors that influence their final properties. These insights are invaluable for the development of advanced CNFs with tailored properties suitable for a range of applications, including but not limited to energy storage, electronics, and as supporting materials in various technological domains.