In this study, gold nanoparticles (AuNPs) were synthesized using the Turkevich method. This article explains the didactic step-by-step synthesis, showing pictures of the entire process, including a well-explained mechanism and characterization study. Synthesis involves the reduction of NaAuCl4 using sodium citrate at high temperatures (approximately 90 °C). The two main mechanisms used to explain AuNPs synthesis via the Turkevich method are also discussed. The first mechanism considers that a nanowire intermediary and the other proposes that aggregate intermediates are not formed at any time during the synthesis. The materials (NaAuCl4 and AuNPs) were characterized using UV-Vis spectroscopy, scanning electron microscopy (SEM), atomic force microscopy (AFM), X-ray diffraction (XRD), and dynamic light scattering (DLS). The UV-Vis spectrum exhibits an absorption maximum at 521 nm because of the surface plasmon resonance (SPR) absorption band of the AuNPs. The SEM images of NaAuCl4 show crystals with cubic shapes, while the AuNPs have an average particle size of approximately 16–25 nm and particles that appear mainly spherical. To confirm the particle shapes, AFM was conducted, and it was possible to clearly observe individual spherical nanoparticles and their aggregates, and the average diameter of these AuNPs was approximately 12–19 nm. The XRD pattern of AuNPs showed four main characteristic peaks corresponding to the (111), (200), (220), and (311) planes, confirming the presence of cubic (FCC) gold. The DLS presented an average particle size of 3.3 ± 0.9 nm and a polydispersity index (PDI) of 0.574. AuNPs were synthesized using a simple and rapid method. The resulting spherical and ultra-small particles can be used in several applications.
In this work, a silver/silver chloride ink is fabricated using two steps. First the silver ink is prepare using silver, nail polish and acetone. Then the silver ink is painted in a paper substrate and a silver chloride layer is deposited using a bleach solution. The result is the silver/ silver chloride conductive ink. The silver ink is cheap ($2.49/g), well-dispersive and very easy to fabricate. The materials were characterized by SEM and XRD. The Ag ink showed the formation of a continuous network throughout the silver ink film with fewer agglomeration.The effective chlorination process was also observed in the Ag/AgCl characterization. Since the Ag/AgCl substrate will be used as a quasi-reference electrode, it is important to investigate the electrical properties. The Ag ink showed an average ohmic resistance of 2.27 Ω. The addition of the AgCl layer decreases the conductivity, as expected. In summary, the Ag/Ag/Cl ink developed is simple, well-dispersed, cheap and with good conductivity. Therefore, it can be used as a conductive ink in the fabrication of quasi-reference electrodes.
The fabrication of the Screen‐Printed Electrode (SPE) was performed using the graphite ink to print the working (WE) and counter electrodes (CE), and silver/silver chloride path as reference electrode (RE). All the electrodes are printed in a paper substrate using screen‐printing technique. The resulting SPE is characterized using scanning electron microscopy, showing all the ink layer, and subsequently optimized. The paper sample presented the cellulose fibers entanglement, extremely rough, with highly porous network. Then the graphite ink was deposited and the surface became flat, thinner and very smooth. When the silver ink was painted on top of the graphite ink, the spherical silver particles, ranged from 2–3.5 μm in size, were observed. And finally, the silver ink was covered with a AgCl layer and the particle size becomes larger with an irregular sphere‐like phase. The images showed that the layers appear to be homogeneously distributed with good coverage. Then fabrication process was optimized concerning type of paper, the sanding process, the hydrophobic barrier, the electrode design and size. In summary, the optimized values included using the previously sanded matte paper with a mineral spirit layer. The design and size of the electrode were also tested to achieve the best electrochemical performance (design 3 with 3.5 cm). The final SPE was a miniaturized and flexible paper‐based electrochemical electrode. In order to evaluate the electrical properties, the ohmic resistance of each ink was tested using a multimeter and the obtained values were 2.18 kΩ for the graphite ink, 2.27 Ω for the silver ink and 38.33 kΩ for the silver/silver chloride ink. That can indicate the good conductivity of each ink used in the fabrication of the electrode and the correct deposition of Ag/AgCl. Finally, the electrode was used to measure the electrochemical response of K4[Fe(CN)6] in different concentrations. Then a calibration curve was obtained from the voltammograms and a linearity was observed between the current and concentration in the range of 0.50–2.00 mM. That indicates that the SPE has potential to be used as a voltammetric electrode.
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