Fe/SiO2 nanocomposite powders were synthesized by the chemical vapor condensation(CVC) process. Phase and microstructures of the as-prepared powders were investigated with CVC experimental parameters by XRD, TEM and VSM. The analysis of XRD patterns revealed that the Fe/SiO2 powders could be produced above 700. With increasing reaction temperature, the XRD peaks became clearer. The size of powders was about 50nm at 1100oC. The Fe/SiO2 powders showed an intricate long-stand structure attributed to their magnetic characteristics. TEM results revealed that the Fe powders were covered by SiO2 layer fully or partially depending on the experimental condition. The saturation magnetization and the coercive force of the as-sytheised powders were investigated with the decomposition temperature.