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In the present work, complex powder alloys containing spinel as a minor phase were produced by mechanical alloying in a high-energy planetary ball mill from a 33Al–45Cu–22Fe (at.%) powder blend. These alloys show characteristics suitable for the synthesis of promising catalysts. The alloying was conducted in two stages: at the first stage, a Cu+Fe powder mixture was ball-milled for 90 min; at the second stage, Al was added, and the milling process was continued for another 24 min. The main products of mechanical alloying formed at each stage were studied using X-ray diffraction phase analysis, Mössbauer spectroscopy, transmission electron microscopy, and energy-dispersive spectroscopy. At the end of the first stage, crystalline iron was not found. The main product of the first stage was a metastable Cu(Fe) solid solution with a face-centered cubic structure. At the second stage, the Cu(Fe) solid solution transformed to Cu(Al), several Fe-containing amorphous phases, and a spinel phase. The products of the two-stage process were different from those of the single-stage mechanical alloying of the ternary elemental powder mixture; the formation of undesirable intermediate phases was avoided, which ensured excellent composition uniformity. A sequence of solid-state reactions occurring during mechanical alloying was proposed. Mesopores and a spinel phase were the features of the two-stage milled material (both are desirable for the target catalyst).

Elimination of Composition Segregation in 33Al–45Cu–22Fe (at.%) Powder by Two-Stage High-Energy Mechanical Alloying