In this paper, porous NiTi alloy prepared by powder metallurgy method was oxidized at high temperature. The effect of oxidation temperature and time on quality of oxidation layer of porous NiTi was studied. The component and morphology of oxidation layer before and after oxidation at high temperature were analyzed by XPS and SEM. The behavior of Ni ion release of porous NiTi alloy was observed. The results showed uniform and thick oxidation layer was formed on the surface of porous NiTi alloy after oxidation at 550°C for 1h. XPS analysis showed the oxidation layer mainly composed of TiO2, and the thickness of the film was about 180nm higher than that before oxidation. The research on the behavior of Ni ion release showed the Ni release after oxidation can be significantly reduced at simulated body fluid due to TiO2 layer.