Abstract. Intermetallic Ni 3 Al-based alloys (doped with zirconium and boron) represent a group of advanced materials with potential outstanding physical and chemical properties (such as high catalytic activity and structural stability in corrosive environments) that make them a considerable candidate for many high-tech applications. In this paper, the catalytic activity of fully dense Ni 3 Albased thin foils (as thin as 50 碌m) possessing structures with micrometer or nanometer grain sizes is discussed. The examined material, without any additional catalytic coating, was successfully produced from as-cast coarse-grained sheets by heavy cold rolling and recrystallisation with an appropriately chosen set of parameters. The examination focuses on methanol and methanol/water mixture decomposition into H 2 and CO at temperatures up to 530 O C in a quartz reactor. Except for these products, a small amount (below 1%) of CO 2 and dimethyl ether was observed. The catalyzed reaction began effectively at about 400 O C, with a methanol conversion of about 90% or higher.