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Two methods for preparing La0.9 K0.1CoO3 perovskite composite oxides, traditional solid state reaction method and sol-gel method, were compared. The characteristics of the powders, such as purity, particle diameter, BET surface area, pore diameter, were investigated by using TG-DTA, XRD, SEM and BET methods. The experimental results show that La0.9 K0.1 CoO3 perovskite composite oxide can be obtained by using the two methods. The purity of La0.9 K0.1CoO3 powders can be increased by raising the calcining temperature while the particle diameter increased and BET surface area decreased. At the same calcining temperature , the properties of the La0.9 K0.1CoO3 powders synthesized by the sol-gel method are superior to those synthesized by the solid state reaction method , such as purer phase, smaller particle diameter , which can be used as a satisfactory catalyst in diesel waste gas cleaning.