The electrospinning technique is a simple and inexpensive method for the manufacture of electrospin nanofibers (ENFs), which can then be converted into carbon nanofibers (CNFs) through two processes. They are namely the usual mixing process and the carbonization process. Controlling the properties of CNFs covering diameter, surface area, porosity during fabrication, makes them superior to other carbon nanomaterials. The purpose of this study was to compare the structural morphology of carbon nanofibers (CNFs) fabricated by electrospinning, with different treatments. Polyvinyl alcohol (PVA) is used as the basic polymer to form nanofibers which will be mixed with activated carbon as CNFs. In this process, PVA has been formed into nanofibers and thermally carbonized at optimal temperatures to form CNFs. Characterizations of structure and morphology are conducted for the resulted CNFs.