A new processing routine which is composed of the chemical disproportion method and heat treatment is used to prepare fine composite powder possessing different microwave absorption properties. The composition, particle size and microwave absorption properties can be easily adjusted by changing the process parameters. The frequency widths below -10 dB of all the specimens are no less than 2.0 GHz. The X-ray diffraction analysis results showed that fine magnetic powder deposited from the reaction solution was amorphous material. They were crystallized after heat treatment. Fine composite powder consists of Fe3Si, Co3C and a little SiC. The greater the amount of polycarbosilane in the mixture, the more the amount of the metal composition in the powder.