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Copper electrodeposition in acidic cupric methanesulfonate electrolyte with organic additives was discussed in this study. The influence of the additives in acidic cupric methanesulfonate bath was studied by means of electrochemical measurement using a rotary electrode and actual TSV copper depositions. The electrochemical parameters including exchange current density and cathodic transfer coefficient of base cupric methanesulfonate electrolyte were successfully determined. Chronoamperometry (CA) was conducted to verify the diffusion time of additives to the surface of electrodes and the corresponding diffusion constants were characterized.