Raney-type catalysts are widely applied in a variety of commercial processes in the chemical industries. Conventionally, Raney nickel catalysts are produced by leaching aluminum from cast Al-Ni alloys; they consist of porous nickel particles having small amounts (3-5 wt. %) of residual aluminum and surface areas in the range of 50-130 m 2 /g [1]. In recent years, reports have been made regarding the production of Raney catalysts by leaching of precursor alloys obtained by mechanical alloying

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... ) [2][3][4]. In these studies, the microstructural characterization has been quite limited in detail. The results of our own work with Raney nickel and nickel-iron catalysts have clearly shown that, compared to conventional Raney catalysts, those derived from precursor alloys prepared by MA possess important advantages regarding simplicity and reproducibility of production, as well as catalytic performance. In order to better understand these findings, we have now conducted a comparative microstructural characterization of conventional and MA Raney catalysts.