The effects of synthesis parameters during the preparation of Ni catalysts for the CO2 methanation reaction via chemical vapor deposition (CVD) were investigated. For this purpose, a central composite design from the design of experiment approach was conducted to identify and investigate the most significant parameters. A surface response methodology was applied to identify promising synthesis parameter combinations that led to highly dispersed Ni catalysts and to understand the interaction of the synthesis parameters. Finally, the methanation activity of a CVD-prepared catalyst was compared with two different Ni catalysts with the same metal loading but prepared with different methods. The CVD preparation herein presented proved to be a promising method to obtain low-loaded Ni catalysts in CO2 methanation. (C) 2018 Institution of Chemical Engineers. Published by Elsevier B.V. All rights reserved.