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The Cu/Co layer film on the sendconductor silicon was obtained by electrodeposition for the first time. The results of current - time transient curves and STM image showed that the wt of Cu film is two-dimensional while an island three-dimension poth for the Co film was formed. The addition of CrO3 changed the current - time transient curves, and affected the growth of crystal. The addition of CrO3 decreased the nucleation rate of Cu, while it changed the shaPe of current-timetransient curves of the deposition of Co at higher deposition potelltials. For the deposition of Co, addition of CrO3 can form the adhesive film [Co. xCr2O3’ YH2O]ad or [CoOH. nCr(OH)3]ad, which decreased the nucleation rate of Co.