Nanocomposites with ZrO2@S-Doped g-C3N4 as an Enhanced Binder-Free Sensor: Synthesis and Characterization.

This study describes new electrocatalyst materials that can detect and reduce environmental pollutants. The synthesis and characterization of semiconductor nanocomposites (NCs) made from active ZrO2@S-doped g-C3N4 is presented. Electrochemical impedance spectroscopy (EIS) and Mott-Schottky (M-S) measurements were used to examine electron transfer characteristics of the synthesized samples. Using X-ray diffraction (XRD) and high-resolution scanning electron microscopy (HR-SEM) techniques, inclusion of monoclinic ZrO2 on flower-shaped S-doped-g-C3N4 was visualized. High-resolution X-ray photoelectron spectroscopy (XPS) revealed successful doping of ZrO2 into the lattice of S-doped g-C3N4. The electron transport mechanism between the electrolyte and the fluorine tin-oxide electrode (FTOE) was enhanced by the synergistic interaction between ZrO2 and S-doped g-C3N4 as co-modifiers. Development of a platform with improved conductivity based on an FTOE modified with ZrO2@S-doped g-C3N4 NCs resulted in an ideal platform for the detection of 4-nitrophenol (4-NP) in water. The electrocatalytic activity of the modified electrode was evaluated through determination of 4-NP by cyclic voltammetry (CV) and differential pulse voltammetry (DPV) under optimum conditions (pH 5). ZrO2@S-doped g-C3N4 (20%)/FTOE exhibited good electrocatalytic activity with a linear range from 10 to 100 µM and a low limit of detection (LOD) of 6.65 µM. Typical p-type semiconductor ZrO2@S-doped g-C3N4 NCs significantly impact the superior detection of 4-NP due to its size, shape, optical properties, specific surface area and effective separation of electron-hole pairs. We conclude that the superior electrochemical sensor behavior of the ZrO2@S-doped g-C3N4 (20%)/FTOE surfaces results from the synergistic interaction between S-doped g-C3N4 and ZrO2 surfaces that produce an active NC interface.

Synthesis and characterization of CuO@S-doped g-C3N4 based nanocomposites for binder-free sensor applications.

This study presents the simultaneous exfoliation and modification of heterostructured copper oxide incorporated sulfur doped graphitic carbon nitride (CuO@S-doped g-C3N4) nanocomposites (NCs) synthesized via chemical precipitation and pyrolysis techniques. The results revealed that the approach is feasible and highly efficient in producing 2-dimensional CuO@S-doped g-C3N4 NCs. The findings also showed a promising technique for enhancing the optical and electrical properties of bulk g-C3N4 by combining CuO nanoparticles (NPs) with S-doped g-C3N4. The crystallite and the average size of the NCs were validated using X-ray diffraction (XRD) studies. Incorporation of the cubical structured CuO on flower shaped S-doped-g-C3N4 was visualized and characterized through XRD, HR-SEM/EDS/SED, FT-IR, BET, UV-Vis/DRS, PL, XPS and impedance spectroscopy. The agglomerated NCs had various pore sizes, shapes and nanosized crystals, while being photo-active in the UV-vis range. The synergistic effect of CuO and S-doped g-C3N4 as co-modifiers greatly facilitates the electron transfer process between the electrolyte and the bare glassy carbon electrode. Specific surface areas of the NCs clearly revealed modification of bulk S-doped g-C3N4 when CuO NPs are incorporated with S-doped g-C3N4, providing a suitable environment for the binder-free decorated electrode with sensing behavior for hazardous pollutants. This was tested for the preparation of a 4-nitrophenol sensor.