This paper describes the surface structure and hydrogenation activity of plate-type Raney iron catalysts. When molten aluminum was sprayed onto surface of iron plate and the plate was heated, an alloy layer was formed at the boundary. Raney iron catalyst was prepared by leaching aluminum from the alloy with an aqueous sodium hydroxide. The characteristics of the alloy phase and the surface of the catalyst were determined by means of an electron probe microanalyzer and X-ray diffractometer. The alloy phase was FeAl3 and Fe2Al5. Catalyst based on alloy from SUS 304 (stainless steel containing 8% Ni and 18% Cr) substrate exhibted greater activity in hydrogenation of acetone than a similar catalyst based on SUS 430 (Stainless steel containing 16% Cr).