Nanoindentation is adopted to study the oxidation evolution of niobium-based alloy at nano-scale at elevated temperatures. An indentation pit at room temperature was created as a “marker” before the temperature was raised to 800 °C. A non-uniform oxide scale on the surface was observed real time by in situ scanning probe microscope. Elastic modulus and hardness obtained at different temperatures exhibit clearly the oxidation effect, which is also demonstrated by creep tests for 600s by using dynamic mechanical analysis of nanoindentation.