Abstract: An unsupported particulate catalyst especially useful for methanation reactions is prepared by a method comprising fluid-bed roasting agglomerates of nickel sulfide to form a particulate precursor material which can be reduced to composite particles consisting essentially of a nickel-oxide core with a then coherent adherent layer of nickel thereon, the reduced particles being characterized at the surface by the presence of microcapillary pores interconnecting with each other and the outer surface of the particles.