The compound SbNbO4 that is formed in a ternary system of NbSbO has been obtained for the rst time by high-energy ball milling of the equimolar mixture of oxides Sb2O3/Nb2O5in argon atmosphere. This compound was characterised by X-ray diraction, dierential thermal analysis-thermal gravimetry, infrared, and scanning electron microscopy methods and its properties were compared with those of SbNbO4 also obtained as a result of high-temperature reaction between the same oxides and also in argon atmosphere. As shown by dierential thermal analysis results, irrespective of the method of synthesis, SbNbO4 is stable in argon atmosphere up to ≈ 1125• C and in air up to ≈ 800• C. The compound can be applied as a photocatalyst in the reaction of producing hydrogen from water.