Abstract: Transition metal nanoclusters of Fe、Co、Ni and Cu have been obtained by Zn reduction in metal-ammonium sulfate solutions. The products were characterized by XRD, SEM, TEM and ED methods. Meantime, the reduction processes have especially been investigated. Experiments indicated that the nanoclusters were observed as solid solutions of displacement by zinc in varying extent. Fe displaced solid solution formed on the surface of zinc particles, however, Ni and Co nanoclusters formed as saturated solid solution with diameter about 7.5 nm and 12.1 nm, respectively. New phase of Cu5Zn8 was observed on the surface of Cu particles. The mechanism of the mentioned processes were discussed and considered as an influence by the driving force of EMF occurred from M-Zn oxidation-reduction cell.

Key words: Nanopowder, Transition metals, Cu₅Zn₈, Solid solution, Zn reduction