A new method of synthesis of nanosized and ultrafine tungsten oxide and carbide powders is offered, which combines carbon carrier supported classical liquid-phase precipitation and low-temperature microwave treatment. The full range of intermediate substances obtained during thermolysis, reduction and carburization of precursors to final products is presented. It is shown that cooling of ammonium tungstate solution to 4 °C and the use of carbon carrier at the precipitation stage can increase the specific surface area from 20 to 100 m 2 g −1.