In this paper, it systematic Study on preparation of multiwalled carbon nanotube (MWCNT)-supported nickel catalyst is pursued. Functional groups are introduced on the surface of MWCNTS using nitric acid, sulfuric acid, and partial oxidation in air. Nickel oxide nanoparticles are formed on the surface of functionalized multiwalled carbon nanotubes by incipient Wetness impregnation of nickel nitrate, followed by calcination in air. The effects of acid type in(] concentration, acid treatment time, partial oxidation, nickel loading, precursor solvent, and calcination temperature Oil the size of the nickel nanoparticles and homogeneity of the composite material are evaluated, Characteristics of the Ni/MWCNT catalysts Were examined using BET, scanning transmission electron microscopy, X-ray diffraction, thermogravimetric analysis in air and nitrogen, temperature-programmed reduction, X-ray photoelectron spectroscopy, acid-base titration, and zeta-potential analyzer. Results of this work are useful Cor formulating CNT-supported nickel catalysts for I wide range of different applications, Such as reforming of hydrocarbons, catalytic hydrothermal gasification of biomass, and energy storage.