SiC/TiO2 microspheres were fabricated using polycarbosilane (PCS) and tetrabutyl titanate as precursors by precipitation technology and polymer derived ceramics route. The effect of operating conditions on the size and surface morphology of PCS/TiO2 microspheres was studied by SEM. The polymer to ceramic conversion and the crystallisation behaviour were studied by thermogravimetry, Fourier transform infrared and X-ray diffraction, suggesting the PCS/TiO2 microspheres converted to the SiC/TiO2 ceramic microspheres through pyrolysis process at different temperatures. At 1200 deg C, the ceramic microspheres were composed of rutile TiO2 and crystalline phases and kept sense spherical shape with crystalline grains at the surface. The ceramic microspheres had an average diameter of 4um, making them promising in infrared shielding applications.