This paper presents the preparation of ultrafine powders of Fe3O4 and Ni by a chemical method, followed by mixing the prepared powders with mica and other ultrafine powders for synthesizing microwave absorption coatings. The microwave attenuation rate of the coatings was measured by the Microwave Network Analyzer in the frequency range of 8-12 GHz at room temperature. The results indicate that microwave could be absorbed by the coatings with an effectiveness strongly dependent on the powder sort and content and the coating thickness. This paper presents the preparation of ultrafine powders of Fe3O4 and Ni by a chemical method, followed by mixing the prepared powders with mica and other ultrafine powders for synthesizing microwave absorption coatings. The microwave attenuation rate of the coatings was measured by the Microwave Network Analyzer in the frequency range of 8-12 GHz at room temperature. The results indicate that microwave could be absorbed by the coatings with a strong resistance dependent on the powder sort and content and the coating thickness.