Cobalt ferrites were prepared by citrate sol-gel method, chemical co-precipitation, mechanical grinding, respectively. The grain size, morphology, and the size of crystal particles were studied by x-ray diffraction (XRD) and scanning electron microscope (SEM). Cobalt ferrite showed different morphologys when prepared by different methods, It was tapered corners which prepared by sol-gel method; It was tetrahedral which prepared by mechanical grinding method; It was sphere which prepared by chemical co-precipitation method. The average grain size of cobalt ferrite was less than 100nm, while particles prepared by chemical precipitation method were the smallest. The size of Cobalt ferrite prepared by sol-gel method was decreased with the cobalt content increased.