The preparation of hydroxyl chromium oxide by hydrogen reduction of disodium chromate and particulate hydroxyl mechanical activation features were studied. Then with self-made hydroxyl chromium as the raw material, a direct reduction and carburization process was used to prepare ultra-fine chromium carbonization. Through SEM and XRD, the high performance mechanical activation, key coefficients, microstructure, hardness and wear-resisting property were investigated. The results reveal that suitable mechanical activation and carbon reducing carbonization temperature, carbonization time, carbon content are beneficial to obtaining ultra-fine chromium carbonization. Typically, when the time of high performance grinding is 5 min, the carbon reducing temperature is 1 100 ℃, the carbon reducing time is 1 h, the carbon content is 28%, and finally the particle size of chromium carbide powder is 1 μm. Under this condition of preparation of ultra-fine chromium carbide, both the hardness and wear resistance are better than those in the industrialization of chromium carbide coating.