Sb 2 Co alloy in powdery form was synthesized via reduction with gaseous hydrogen of the oxide CoSb 2 O 6 , obtained by the citrate gel-combustion technique. The precursor was an aqueous solution of antimony nitrate, cobalt nitrate and citric acid. The precursor solution with mole ratio Co(II)/Sb(V) of 1:2 was gelatinized by evaporation of water. The gel was heated in air up to the temperature of self-ignition. The product of gel combustion was a mixture of oxides and it had to be additionally thermally treated in order to be converted to pure CoSb 2 O 6 . The reduction of CoSb 2 O 6 by gaseous hydrogen yielded powdery Sb 2 Co as the sole phase. The process of oxide reduction to alloy was controlled by thermogravimetry, while X-ray diffractometry was used to control the phase compositions of both the oxides and alloys.