In this study, Cu and Co doped Ni/Al2O3 nanocatalyst was synthesized via impregnation and sol–gel methods. The physiochemical properties of nanocatalyst were characterized by XRD, field emission scanning electron microscopy (FESEM), particle size distribution, BET, fourier transform infrared spectroscopy (FTIR), TG–DTA and energy dispersive X-ray (EDX) analysis. The samples were employed for CO2-reforming of methane in atmospheric pressure, temperature range from 550 to 850 °C, under various mixture of CH4/CO2 and different gas hourly space velocity. XRD patterns besides indicating the decline of the peaks intensity in sol–gel method, proved the potential of this procedure in diminishing the crystal size and preventing the NiAl2O4 spinel formation. Moreover, high surface area might derive of smaller particle size and uniform morphology of sol–gel prepared ones, confirmed by FESEM and BET analysis. TG–DTG analysis as well supported the higher surface area for sol–gel made ones, represented the proper calcination temperature (approximately 600 °C). Also, presence of the active phases and elemental composition of nanocatalysts determine via EDX analysis. Promoting the basicity and the adsorption rate of CO2, is attributed to the higher amount of OH groups for sol–gel prepared samples, proved by FTIR. Ni–Co/Al2O3 due to the synergetic effect of sol–gel method and cobalt addition depicted excellent characterization such as higher surface area, smaller particle size, supplying more stable support and enhanced morphology. Therefore, this nanocatalyst represented the best products yield (H2 = 98.21 and CO = 95.64), H2/CO close to unit (0.92–1.05) and stable conversion during 1,440 min stability test. So, Ni–Co/Al2O3 among all of the prepared nanocatalysts demonstrated the best catalytic performance and presented it as a highly efficient catalyst for dry reforming of methane. Despite of the stable yield of Ni–Cu/Al2O3, it depicted the lower catalytic activity and H2/CO ratio
