<p>The conversion of CO₂ to CH₄ is a promising technology for future generation survival. CH₄ is a clean-burning fuel that provides a way to store renewable energy. A series of Ni and Fe supported Alumina catalysts were prepared by coprecipitation method with 15&#xa0;wt.% of Ni, Fe, (75Ni–25Fe) metal loading, characterized by H₂-TPR, XRD, CO₂-TPD, H₂-TPD techniques and studied by in-situ Diffuse Reflectance Fourier-Transformed Infrared (DRIFT) spectroscopy during the CO₂ adsorption and hydrogenation reaction and the catalytic action of the prepared catalysts was performed in a system in the form of pulses operating under differential conditions at atmospheric pressure. It is crucial because it prevents the catalyst from being overloaded with gas, which can lead to inaccurate results. It revealed that the amount of CO₂ adsorbed estimated from CH₄ formed and calculated the conversion and Space–Time Yield (STY). For bimetallic catalysts, the STY is 1.2 times higher and almost 2 times better conversion at a lower temperature (300&#xa0;°C) compared to the monometallic catalysts. The peak temperature of CH₄ formation over the bimetallic catalyst is observed at a low temperature when compared to the monometallic catalysts, indicating that methanation proceeds faster on the bimetallic catalyst. It is suggested that adding Fe to Ni leads to a decrease in the rate of CO₂ dissociation, which is thought to be an essential step in the methanation reaction. This study also revealed that the 15(Ni–Fe)/Al₂O₃ catalyst has a lower activation energy of 0.73 times than the 15Ni/Al₂O₃ catalyst so the reaction can proceed more easily on the 15(Ni–Fe)/Al₂O₃ catalyst at 1.15 times lower temperatures than the prepared catalysts. The findings in this work are expected to offer a more reasonable explanation for previous studies and provide guidance for future reaction design.</p>