Processes occurring in synthesis of a-Fe from a Fe(III) solution using an aluminum matrix were studied. The reaction kinetics strongly depends on the state of the matrix.Dispersed and ultradispersed iron metal and its alloys are widely used in various branches of science and engineering thanks to their unique magnetic, mechanical, catalytic, and other properties. The properties of these materials largely depend on the procedure of their preparation. It should be noted that the known processes for reduction of Fe(III) from aqueous solutions are very few and often do not ensure high yield of iron metal under normal conditions. Also, it is known that the history of iron metal preparation appreciably affects its physical and chemical properties, which should be taken into account in preparation of materials with preset characteristics.Metal formulations with an aluminum matrix attract much researchers' attention [135]. Thanks to a unique combination of protective properties of surface oxide3hydroxide layers and intrinsic chemical activity, aluminum under definite conditions chemically reacts with the surrounding medium to form compounds exhibiting a series of specific properties [6,7]. According to numerous papers, finely dispersed aluminum powder considerably surpasses compact aluminum in the chemical activity toward water and aqueous solutions of various compounds [8,9]. It is believed [6,8,9] that this is due to the developed surface of the powders, to strongly defective state of the surface oxide3hydroxide films on fine particles, and to strong heat-up of the solid phase in the course of oxidation [9]. These factors can appreciably affect the course and extent of the reaction of finely dispersed and compact aluminum with an aqueous solution containing metal ions. It should be noted, however, that we found no detailed information on the reduction of Fe(III) ions with aluminum in solution. In this connection, it seems important to study how the aluminum matrix affects the redox process involving reduction of Fe(III).Our goal was to elucidate the mechanism of the reaction of compact and dispersed (with different particle size) aluminum with an aqueous solution of Fe(III) chloride and to reveal characteristic kinetic features of separate steps of the process.