One of the major factors for global warming is the increase in the concentration of CO2 in the atmosphere. There are several reserves of natural gas available in Malaysia that contain various other hydrocarbons; however, they are rendered useless due to the high concentration of CO2. There have been studies where CO2 is being utilized in the production of syngas, in which catalysts employed for the synthesis mainly consist of transition metals such as Fe, Ni, Al, Mg, and Mo. In this study, Fe and Ni hydrotalcites catalysts were prepared by co-precipitation method. Al2NO3, MgNO3, and NiNO3 were titrated dropwise against Na2CO3.10H20 while maintaining the temperature and the pH of the solution at 70oC and pH 10, respectively. Similarly, for the iron catalyst, the NiNO3 was replaced with FeNO3 and the remaining chemicals were varied according to the stoichiometric parameters. The catalyst produced was then vacuum-filtered, dried at 80oC and calcined at 650oC. The calcined catalyst was used in the reactor. The gases produced were analyzed using gas chromatography and showed that H2 gas was being produced, finally after the reaction was completed the used catalyst was analyzed by Field Emission Scanning Electron Microscope (FESEM) to prove the growth of carbon nanomaterial. © Malaysian Journal of Microscopy (2020). All rights reserved.