Cobalt-phthalocyanine/iron nanocomposite particles have been obtained using method of composite in situ, with the mixture of carbonyl iron and solution of cobalt ( Ⅱ ) - phthalocyanine (Co-Pc) ultrasonic dispersing in N,N-dimethyl-formamide (DMF). Structure characterization of their inner and surface have relation with method of carbonyl iron joined in the mixture, contents of carbonyl iron and Co-Pc in the mixture of Co-Pc ultrasonic dispersing in DMF. With a method of composite in situ controlling reasonable experiment condition, it can be obtained that cobalt-phthalocyanine/iron nanocomposite particles has completely been covered with Co-Pc, they had structure of Chinese gooseberry in inner and mere made up of almost regular spherical shape and the average diameter is 1. 4 μm.