One-pot electrodeposition of multilayered 3D PtNi/polymer nanocomposite. H2O2 determination in aerosol phase

In this work, 3D-structured nanocomposites were synthesized in one pot by electrochemical deposition of alternating layers of an azo type polymer (polyazure-A) with platinum and nickel nanoparticles. The hybrid PtNi/poly(AzA) film was electrochemically deposited on screen-printed carbon electrodes by layer-by-layer assembly as a function of the number of cyclic voltammograms for electrodeposition of the conducting polymer and the electrode potential applied for electro-reduction of the metal salts. The physicochemical characteristics of the resulting films were studied using electrochemical and microscopic techniques. The 3D molecular nanoarchitecture presents a hollow porous structure dependent on the electrode potential set for the electro-reduction of Pt and Ni nanoparticles. The electrochemical sensor was validated in terms of sensitivity, limit of detection, stability and repeatability, exhibiting a highly sensitive H2O2 detection, with LoD 68.5 nM (S/N = 3) at 0.05 V vs. Ag-SPCE for the electrode modified with 20 cycles for the conducting polymer electrodeposition and −2.0 V for metal ions reduction. The aim of this work also included the outcome of the electrochemical sensor after incorporating the room temperature ionic liquid 1‑butyl‑2,3-dimethylimidazolium tetrafluoroborate within the PtNi/poly(AzA) film, which notably improved the analytical parameters of the system, with LoD 14.5 nM at the same potential. Therefore, as proof of concept, the PtNi/poly(AzA) film-based electrode was explored towards the suitability of an electrochemical sensor for the determination of hydrogen peroxide in aerosol phase. The outstanding features of the PtNi/poly(AzA) film-based electrode modified with the aforementioned ionic liquid allowed for the continuous monitoring of H2O2 in an aerosol stream generated with an ultrasonic diffuser at the low applied potential of 0.05 V. In addition, monitoring H2O2 samples through a series of ON/OFF switches for over 3 h, the sensor provided a fast and reproducible response.