Ultra-fine Ti(C,N)-Mo2C-Ni cermets powders were prepared by sol-gel method and carbon thermal reduction method. The orthogonal experiment was designed to study the preparation process. The structure and morphology of the powders prepared under the best technology were analyzed through the detection means of X-ray diffraction (XRD) and scanning electron microscopy (SEM). The research results showed that: when the pH was 4, H2O and Ti(OBu)4 molar ratio was 6:1, Sucrose and Ti(OBu)4 was 4:1 and the drying temperature was 60℃, minimum powder grain was obtained with the shape into a block and the particle size of 150~2 000 nm, and the gel time was short.