In this study, we succeeded in synthesizing polyacrylic acid in a double-current two-phase cell system containing water and ethyl acetate on a Cu electrode. The more detailed steps for grafting polymerization of acrylic acid on the copper electrode are as follows: (1) Electrochemical reduction of p-dinitrobenzene (DNB) to 4- nitroaniline (4NA) in ethyl acetate by applying a potential of −0.1 V vs Ag/AgCl. (2) Conversion of 4NA to corresponding diazonium cation through its reaction with NaNO2 in the aqueous phase. (3) Electrochemical generation of Cu+ from Cu electrode in the aqueous phase. (4) Reduction of diazonium cation by Cu+ and formation of aryl radical and (5) polymerization of acrylic acid on copper electrode initiated by aryl radicals. The structural properties and characteristics of the deposited polyacrylic acid layer is fully characterized using different spectroscopic techniques, electrochemical and surface analysis studies. The present method is efficient (82.2 % AE) and the experimental results confirm our strategy in creating an attractive architecture of a non-porous insulating film on the electrode surface.
