Abstract Material science could be considered as an emerging route for finding suitable catalysts applying in different fields. In this investigation, LaNiO 3 was prepared by co‐precipitation. The influence of the heat treatment conditions (temperature and duration) on potential LaNiO 3 perovskite material was presented herein this report. The characteristic properties of LaNiO 3 were elucidated via several techniques, including XRD, EDS, SEM, HR‐TEM, H 2 ‐TPR, CO 2 ‐TPD, and isotherm N 2 adsorption. CO 2 methanation was used as a means for measuring the catalytic applicability of the studied materials. The results showed that the thermal stability of the perovskite material prohibited the growth of crystallite sizes and prevented the crystallite sizes from significantly changing. Nevertheless, the variation of temperatures and durations in calcination and reduction processes led to different H 2 consumption behavior and CO 2 desorption amounts. The reduction conditions were found to have a significant impact on the catalytic activity of reduced LaNiO 3 in CO 2 methanation, which might have a close correlation to the basicity of as‐reduced LaNiO 3 . The research results determined that the most appropriate calcination and reduction conditions of LaNiO 3 to produce the best Ni/La 2 O 3 catalyst are 650 °C (2 h) and 500 °C (2 h), respectively. Findings confirmed that via the co‐precipitation method and moderate temperatures, it was possible to prepare a highly dispersed Ni catalyst, dispersed on La 2 O 3 /La(OH) 3 of relatively large specific surface area, possessing high oxygen vacancies and high basicity provides activity comparable to the best referenced perovskite‐based catalysts. This work laid a useful foundation for further improvement in the synthesis method and changing the catalyst composition to create perovskite catalysts with high methanation efficiency.