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Titanium oxide (TiO2) coated polyimide has broad application prospects under extreme conditions. In order to obtain a high-quality ultra-thin TiO2 coating on polyimide by atomic layer deposition (ALD), the polyimide was activated by in situ oxygen plasma. It was found that a large number of polar oxygen functional groups, such as carboxyl, were generated on the surface of the activated polyimide, which can significantly promote the preparation of TiO2 coating by ALD. The nucleation and growth of TiO2 were studied by x-ray photoelectron spectroscopy monitoring and scanning electron microscopy observation. On the polyimide activated by oxygen plasma, the size of TiO2 nuclei decreased and the quantity of TiO2 nuclei increased, resulting in the growth of a highly uniform and dense TiO2 coating. This coating exhibited excellent resistance to atomic oxygen. When exposed to 3.5 × 1021 atom cm−2 atomic oxygen flux, the erosion yield of the polyimide coated with 100 ALD cycles of TiO2 was as low as 3.0 × 10−25 cm3/atom, which is one order less than that of the standard POLYIMIDE-ref Kapton® film. [ABSTRACT FROM AUTHOR]