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In the toluene solution of the precursor Polycarbosilane (PCS) containing low- molecular-mass additive Ti(OC4H9)4, TiO2/SiC nanometer-scale functional compositional film with the surface TiO2 layer on CF was formed in situ by means of polymer-derived precursors. The effects of Ti (OC4H9)4 concentrations and the maturating time were studied on the densification and TiO2 particle size of surface layer. The compositions of film were TiO2 and SiC crystal by XRD. According to the results of ESCA analysis, Ti(OC4H9)4 compound oozed gradiently from the pre-ceramic PCS to the surface layer after maturating time of 100 h. In the conditions of 45wt% Ti (OC4H9)4 and 100 h maturation, the nanometer-scale TiO2 particles on continuous surface layer were formed by SEM photographs. The nanometer-scale TiO2/SiC functional compositional film can modify the resistance to oxidation of carbon fiber.