Polyimide/titania (PI/TiO2) composite was synthesized by in situ sol-gel polymerization, and carbon/titanium carbide (TiC) composite films were prepared by carbothermal reduction of the PI/TiO2 composite at 1,600 A degrees C under flowing argon. The structure and properties of the composites were studied by wide angle X-ray diffraction (WAXD), Fourier transform infrared spectrometer (FTIR), scanning electron microscopy, and energy dispersive X-ray spectroscopy. The carbon/TiC composite films exhibited metallic luster on the surface and compact structure in cross section with well dispersed TiC particles. WAXD intensity distribution revealed that TiC particles formed by tightly bonding between elemental carbon and titanium formed crystallites which as a filler provided tough films. The results indicated that heat treatment of PI/TiO2 under argon is a promising method for preparing tough carbon composite films.