This study aims to investigate the suitability of methanol as a carbon source for the synthesis of carbon nanofibres (CNFs), currently used in wastewater, water, and air purification systems, by chemical vapor deposition (CVD) in the presence of NiO catalyst. Experimental studies were carried out in a tube furnace under isothermal conditions. Catalyst particles were loaded onto silicon wafers with orientation by dip coating to grow CNFs. The reduction behavior of nickel oxide powder at 1000 K under non-isothermal and isothermal conditions was investigated before CNF synthesis studies. The percentage reduction of nickel oxide powder under non-isothermal conditions was 82.03%. The percentage reduction under isothermal conditions for 30 min was 78.03%. The experimental result obtained is very close to the theoretical value (78.57%). During CNF synthesis experiments, it was observed that CNF formation was not achieved at temperatures of 1000 - 1100 K due to the poor thermal decomposition of methanol. Pyrolysis of methanol increased with increasing synthesis temperature (1200 K), which promoted the synthesis of CNFs. SEM analysis revealed morphologically dense CNF formation under isothermal conditions for 20 min at 1300K synthesis temperature.