The preparation of submicrometer nickel and copper powders by low-temperature pyrolysis of their formate salts in inert atmosphere was studied. Thermoanalytical investigation of nickel and copper formate salts decomposition was done to find out the conditions for metal powders production. Full decomposition of these salts occurs at a temperature range of 200–300 °C. The nickel and copper particles size was shown to depend on the operating conditions, such as: preliminary milling, different additives, temperature and time of pyrolysis, etc. Pure copper and nickel powders with mean particle size of 0.4–0.6 μm were produced.