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A high-throughput method was applied to study oxidation behavior of Nb–Si based alloy using composition spread alloy film as combinatorial libraries. An extended range of composition gradients of Nb–Si based alloy film was deposited by (multi)magnetron co-sputtering. The as-deposited film was composed of amorphous phase. Cr2Nb, Nb5Si3 and Nbss could be detected after annealing treatment. After oxidation at 1250 C for 10 min and 20 min, the film composition space was divided into three regions of the distinct oxide scales. The compositions for establishment of the different oxides on Nb–Si based alloy was defined efficiently across the entire composition space by the combinatorial libraries.