The dry reforming of methane was carried out using a NiV/Al₂O₃ catalyst synthesised by a polymeric precursor method. The composition of the reaction mixture (CH₄/CO₂ ratio) and the temperature were altered to verify the ideal conditions for conversion of methane and carbon. The composition of the syngas formed in the process and the type of carbon deposited on the catalyst were also investigated. The material was characterised by X-ray diffraction (XRD) and temperature-programmed reduction (TPR-H₂). After the catalytic tests were performed, Raman spectroscopy and temperature-programmed oxidation (TPO) analyses were conducted. The results of the catalytic tests show that at elevated temperatures and high CH₄/CO₂ ratios, it is possible to observe a high value for the conversion of methane and carbon dioxide with a H₂/CO ratio greater than unity. The TPO and Raman analyses pointed to catalytic deposition of a large amount of coke that is composed of multiwall carbon nanotubes and amorphous carbon.