The electrochemical growth of carbon nanotubes (CNTs) -conducting polymer composites offers the ability to produce three-dimensional nanostructured films that combine the redox pseudo-capacitive charge storage mechanism of conducting polymers with the high surface area and conductivity of CNTs [1 -3]. In this paper we report the electropolymerization and characterization of polypyrrole films (PPy) doped with poly (m-aminobenzenesulfonic acid) (PABS) functionalized single-walled carbon nanotubes (SWCNTs) (PPy/CNTs). The negatively charged CNTs served as anionic dopant during the electropolymerization to synthesize PPy/CNTs composite films. Electrochemical impedance spectroscopy (EIS), cyclic voltammetry (CV) and scanning electron microscopy (SEM) were used to investigate the electrochemical properties of the composite films.
This article reports an amperometric glucose biosensor based on a new type of nanocomposite of polypyrrole (PPY) with p-phenyl sulfonate-functionalized single-walled carbon nanotubes (SWCNTs-PhSO3−). An environmentally friendly functionalization procedure of the SWCNTs in the presence of substituted aniline and an oxidative species was adopted. The nanocomposite-modified electrode exhibited excellent electrocatalytic activities towards the reduction or oxidation of H2O2. This feature allowed us to use it as bioplatform on which glucose oxidase (GOx) was immobilized by entrapment in an electropolymerized PPY/SWCNTs-PhSO3− film for the construction of the glucose biosensor. The amperometric detection of glucose was assayed by applying a constant electrode potential value necessary to oxidize or reduce the enzymatically produced H2O2 with minimal interference from the possible coexisting electroactive compounds. With the introduction of a thin film of Prussian blue (PB) at the substrate electrode surface, the PPY/GOx/SWCNTs-PhSO3−/PB system shows synergy between the PB and functionalized SWCNTs which amplifies greatly the electrode sensitivity when operated at low potentials. The biosensor showed good analytical performances in terms of low detection (0.01 mM), high sensitivity (approximately 6 μA mM−1 cm−2), and wide linear range (0.02 to 6 mM). In addition, the effects of applied potential, the electroactive interference, and the stability of the biosensor were discussed. The facile procedure of immobilizing GOx used in the present work can promote the development of other oxidase-based biosensors which could have a practical application in clinical, food, and environmental analysis.
We have investigated the influence exerted by the concentration of graphene oxide (GO) dispersion as a modifier for screen printed carbon electrodes (SPCEs) on the fabrication of an electrochemical biosensor to detect DNA hybridization. A new pretreatment protocol for SPCEs, involving two successive steps in order to achieve a reproducible deposition of GO, is also proposed. Aqueous GO dispersions of different concentrations (0.05, 0.1, 0.15, and 0.2 mg/mL) were first drop-cast on the SPCE substrates and then electrochemically reduced. The electrochemical properties of the modified electrodes were investigated after each modification step by cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS), while physicochemical characterization was performed by scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), and Raman spectroscopy. Finally, the sensing platform was obtained by the simple adsorption of the single-stranded DNA probe onto the electrochemically reduced GO (RGO)-modified SPCEs under optimized conditions. The hybridization was achieved by incubating the functionalized SPCEs with complementary DNA target and detected by measuring the change in the electrochemical response of [Fe(CN)6]3–/4– redox reporter in CV and EIS measurements induced by the release of the newly formed double-stranded DNA from the electrode surface. Our results showed that a higher GO concentration generated a more sensitive response towards DNA detection.
In this work, we combine two widely used techniques to produce modified electrodes, that is, the electroreduction of diazonium salts and the electropolymerization of conductive polymers in order to obtain polyaniline (PANI)/carbon nanotube (CNTs) composites. Thus, in a first step, a CNTs electrode was functionalized with 4-nitrophenyl group by electrochemical reduction of 4-nitrobenzenediazonium salt in nonaqueous media. Then, the nitro group was reduced electrochemically to amine functionality. Cyclic voltammetry and electrochemical impedance spectroscopy were used to trace the reactions in each step. The PANI film can easily be grafted onto the surface of such obtained aminophenyl-modified CNTs electrodes. The PANI/CNTs films generated by this strategy show electrochemical behavior similar to that of PANI simply electrodeposited on CNTs electrodes, but exhibit significantly improved stability and higher capacitance values.
In this paper we report the functionalization of conductive polypyrrole (PPY) films via electrochemical reduction of the aryl diazonium salts in a manner that is similar to the one employed for other conductive surfaces. To understand the general trends of the grafting behavior of diazonium salts and to establish the optimal conditions for the covalent functionalization of the PPY films, we have compared the grafting behavior of four p-substituted phenyldiazonium salts: p-nitrophenyl diazonium tetrafluoroborate (PNBDBF 4 − ), p-tolyl diazonium tetrafluoroborate (TDBF 4 − ), p-fluorophenyl diazonium tetrafluoroborate (FPDBF 4 − ) and 4-diazo-N,N-dimethylaniline tetrafluoroborate (DDMABF 4 − ). The selection of the molecules to be grafted was done both for their electroactivity after grafting and the contrasted electronegativityof the substituents at the benzene ring. For all investigated diazonium salts, a linear relationship between their reduction potential at the PPY electrodes and Hammett substituent constants was obtained, suggesting a similar electrochemical reaction mechanism. The functionalization of the polypyrrole films has been evaluated using electrochemical methods like EQCM, CV and EIS. The presence at the polymeric films surface of the functional groups introduced by the electrochemical reduction of diazonium salts was evidenced also by XPS. This approach enables new functionalities on PPY that could otherwise not withstand the polymerization conditions.
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