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In this study the advantages of the electrochemical approach to the formation of polymer/metal nanoparticle composites are demonstrated. The method enables one to simplify the multistage processes of traditional technologies for the production of such materials through combining all intermediate processes in one stage and reducing the total formation time to 3–10 min. The possibility of a single-stage formation of a polymethylolacrylamide/AuNPs composite through including AuNPs into an electrically non-conducting polymethylolacrylamide film (carrier) formed by electropolymerization through potentiostatic electrolysis is also demonstrated for the first time. It is established that the addition of tetrachloroauric acid (HAuCl4·4H2O) into a monomeric composition containing acrylamide, formaldehyde, N,N′-methylene-bis-acrylamide, zinc chloride, and H2O results in simultaneous electrochemical initiation of polymerization with the formation of a polymer film on the cathode, electrolytic reduction of gold ions to Au0, and immobilization of AuNPs particles into the growing polymer matrix. It was found that the formation of the PMAA / AuNPs composite is energetically more favorable than the synthesis of the main PMAA film, since it proceeds at a lower cathodic potential. The inclusion of AuNPs into the polymethylolacrylamide film was confirmed visually, as well as by X-ray phase analysis, small-angle X-ray scattering, microscopy, and element analysis. The gold content in the composite increases along with the increase of the concentration of HAuCl4 in the electrolyte. The radius of the AuNPs particles was found to range between 3 and 7 nm. The AuNPs particles are spherical in shape and can combine into larger clusters containing up to 10 or more particles. The dynamics of formation, structure, and morphology of the polymethylolacrylamide/AuNPs composite were investigated. It was revealed that gold nanoparticles are mainly concentrated in the near-electrode and near-solution layers of the composite. We found that the composite has electrocatalytic activity. The possibility of its use as a sensor for hydrogen peroxide is demonstrated.

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