Glow discharge plasma was applied to substitute thermal calcination during catalyst preparation. Evolution of cobalt particles in cobalt-ruthenium based catalysts at different stages (fresh prepared, reduced, after Fischer-Tropsch synthesis (FTS) reaction) were studied using a series of characterization techniques. Glow discharge plasma can be developed as an efficient technique to decompose metal salt. Cobalt dispersion was greatly enhanced by glow discharge plasma treatment, and higher initial cobalt dispersion was found on the one with lower treating intensity. However, cobalt crystallites generated by plasma treatment below certain intensity had poor thermal stability, they were tended to aggregate into large particles during reduction and reaction processes, and thus severe deactivations were observed during FTS tests. Besides cobalt sintering, mass transfer limitation at high FTS activity due to the pore plugging by long-chain hydrocarbons was also one of the important reasons for deactivation. The CRS-P140 catalyst with higher plasma treating intensity combined relatively high cobalt dispersion, high cobalt reducibility and relatively stable cobalt distribution during reduction or reaction, showed a high FTS activity with less activity loss. (C) 2019 Elsevier Inc. All rights reserved.