The thermal decomposition of metal formates in the production of ultrafine metal powders permits controlling particle size and specific surface S sp , i.e., controlling free surface energy [1,2]. It is believed [3] that the smaller the particles and the more developed the surface, the more nonequilibrium their state and the higher their activity in subsequent pressing and sintering. In turn, this activity reveals itself when thermal and mechanical loads on these powders are low.This paper examines how the process of producing double formate mixtures and thermal decomposition modes affect the composition, particle size, and physical and chemical properties of ultrafine powders.Two methods were employed to produce double powder mixtures (nickel + copper, nickel + cobalt, copper + cobalt) containing components in different ratios, %: 10 + 90, 25 + 75, 50 + 50, 75 + 25, and 90 + 10. The first method involved obtaining pure metal formates, their careful mechanical mixing until they are uniform, and thermal decomposition. The second method involved obtaining formates in the form of solid solutions (or formate of a mixture) with a needed ratio of components, and their thermal decomposition [2].The production of pure metal formates and solid-solution formates is based on the precipitation of basic carbonates or hydroxides of these metals, their subsequent dissolution in the equimolecular amount of formic acid, and sedimentation of practically insoluble formates from the oversaturated solutions. Nickel and cobalt nitrates and copper sulfate are starting compounds for obtaining pure metal formates. Excess sodium carbonate is added to the solution of appropriate salts at 50-60ºC and vigorously mixed to precipitate basic metal carbonates according to the following reactions: 2Ni