The 80Ni20Co/SiO2 catalysts prepared using co-precipitate and incipient wetness impregnation method were used for production of methane through CO2 methanation reaction between CO and H2 gases. The effect of a range of calcination temperature on the structure and catalytic performance of 80Ni20Co/SiO2 catalyst was investigated using microactivity fixed bed reactor. It was found that the catalyst calcined at 400°C for 4.5 h under air atmosphere has shown the best catalytic performance for CO2 methanation. Characterization of 80Ni20Co/SiO2 catalyst calcined fresh samples was carried out using TPR-H2 analysis, Brunauere Emmette Teller (BET) measurements and X-ray diffraction (XRD. It was observed that calcination temperature influenced the structure, morphology and catalytic performance of the catalysts.