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The effect of polyethylene glycols upon copper electrodeposition in methanesulfonate electrolytes is discussed in this paper. By means of linear sweep voltammetry and electrochemical impedance spectroscopy, it is found that polyethylene glycols in methanesulfonat electrolytes have very different behavior from that in traditional sulfuric electrolytes. PEG can adsorb on electrode surface in absent of chloride ion. The presence of chloride would destroy PEG adsorption to the electrode surface. The impedance shows that PEG can inhibit the reactions Cu2+→Cu+ and Cu+→Cu. The special effect of PEG in methanesulfonate electrolyte is probably related to methanesulfonic radical.