This work presents a study of the formation mechanism of electrochemically deposited alternating layers of azopolymer and graphene oxide, as well as a systematic study of the physicochemical characteristics of the resulting nanocomposite films by electrochemical impedance spectroscopy. The nanocomposite films were constructed by cyclic electropolymerization, which allowed for the assembly of thin films with alternating azopolymers and reduced graphene oxide (rGO) layers in one step. Morphological characterizations were performed by atomic force microscopy and scanning electron microscopy and verified that the electrodeposition of the poly(azo-BBY) polymeric film occurred during the anodic sweep, and the deposition of graphene oxide sheets took place during the cathodic sweep. By analyzing the electrochemical impedance spectra using equivalent circuit models, variations in the resistance and capacitance values of the system were monitored as a function of the amount of electrodeposited material on the fluorine doped tin oxide electrode. In addition, the interfacial phenomena that occurred during the electroreduction of the rGO sheets were monitored with the same method.

The use of graphene and its derivatives in the development of electrochemical sensors has been growing in recent decades. Part of this success is due to the excellent characteristics of such materials, such as good electrical and mechanical properties and a large specific surface area. The formation of composites and nanocomposites with these two materials leads to better sensing performance compared to pure graphene and conductive polymers. The increased large specific surface area of the nanocomposites and the synergistic effect between graphene and conducting polymers is responsible for this interesting result. The most widely used methodologies for the synthesis of these materials are still based on chemical routes. However, electrochemical routes have emerged and are gaining space, affording advantages such as low cost and the promising possibility of modulation of the structural characteristics of composites. As a result, application in sensor devices can lead to increased sensitivity and decreased analysis cost. Thus, this review presents the main aspects for the construction of nanomaterials based on graphene oxide and conducting polymers, as well as the recent efforts made to apply this methodology in the development of sensors and biosensors.

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