In the present work, nickel silica composite powder was prepared using an ammoniaammonium sulfate system. Optical microphotographs showed that the coated nickel layer was dense and complete. Suitable operation conditions were reported. The composite nickel viscose fiber prepared by this plating system was also investigated. The mechanism of nickel coating on spherical silica particles and viscose fibers by hydrazine reduction was studied. It was found that tiny Pd spots on the surface of particles or fibers acted as active centers for nickel deposition at the initial stage of the process. Thereafter, Ni itself would act as an active center for catching Ni from the solution through the reaction Ni 2+ + 2H ad * fi Ni + 2H + . The rate of the process was found to be controlled by the reaction at the interface, under the present experimental conditions. Kinetic models were proposed on the basis of the experimental results. The model predictions were found to be in agreement with the experimental data.