Sb2Co alloy in powdery form was synthesized via reduction with gaseous hydrogen of the oxide CoSb2O6, 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 CoSb2O6. The reduction of CoSb2O6 by gaseous hydrogen yielded powdery Sb2Co 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.
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