In line with current research goals involving water splitting for hydrogen production, this work aims to develop a noble-metal-free electrocatalyst for a superior hydrogen evolution reaction (HER). A single-step interfacial activation of Ti3C2Tx MXene layers was employed by uniformly growing embedded WS2 two-dimensional (2D) nanopetal-like sheets through a facile solvothermal method. We exploited the interactions between WS2 nanopetals and Ti3C2Tx nanolayers to enhance HER performance. A much safer method was adopted to synthesize the base material, Ti3C2Tx MXene, by etching its MAX phase through mild in situ HF formation. Consequently, WS2 nanopetals were grown between the MXene layers and on edges in a one-step solvothermal method, resulting in a 2D-2D nanocomposite with enhanced interactions between WS2 and Ti3C2Tx MXene. The resulting 2D-2D nanocomposite was thoroughly characterized using X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), Raman, Fourier transform infrared (FTIR), and X-ray photoelectron spectroscopy (XPS) analyses before being utilized as working electrodes for HER application. Among various loadings of WS2 into MXene, the 5% WS2-Ti3C2Tx MXene sample exhibited the best activity toward HER, with a low overpotential value of 66.0 mV at a current density of -10 mA cm-2 in a 1 M KOH electrolyte and a remarkable Tafel slope of 46.7 mV·dec-1. The intercalation of 2D WS2 nanopetals enhances active sites for hydrogen adsorption, promotes charge transfer, and helps attain an electrochemical stability of 50 h, boosting HER reduction potential. Furthermore, theoretical calculations confirmed that 2D-2D interactions between 1T/2H-WS2 and Ti3C2Tx MXene realign the active centers for HER, thereby reducing the overpotential barrier.
Incorporating the molecular organic Lewis acid tris(pentafluorophenyl)borane [B(C6F5)3] into organic semiconductors has shown remarkable promise in recent years for controlling the operating characteristics and performance of various opto/electronic devices, including, light‐emitting diodes, solar cells, and organic thin‐film transistors (OTFTs). Despite the demonstrated potential, however, to date most of the work has been limited to B(C6F5)3 with the latter serving as the prototypical air‐stable molecular Lewis acid system. Herein, the use of bis(pentafluorophenyl)zinc [Zn(C6F5)2] is reported as an alternative Lewis acid additive in high‐hole‐mobility OTFTs based on small‐molecule:polymer blends comprising 2,7‐dioctyl[1]benzothieno [3,2‐b][1]benzothiophene and indacenodithiophene–benzothiadiazole. Systematic analysis of the materials and device characteristics supports the hypothesis that Zn(C6F5)2 acts simultaneously as a p‐dopant and a microstructure modifier. It is proposed that it is the combination of these synergistic effects that leads to OTFTs with a maximum hole mobility value of 21.5 cm2 V−1 s−1. The work not only highlights Zn(C6F5)2 as a promising new additive for next‐generation optoelectronic devices, but also opens up new avenues in the search for high‐mobility organic semiconductors.
This work presents a hydrothermal-based facile method for synthesizing ZnFe2O4, whose size can be controlled with the concentration of sodium acetate used as a fuel and its physical changes at nanoscales when exposed to two different gases. The structural, morphological, compositional, and electronic properties of the synthesized samples are also presented in this paper. The crystal structure of the synthesized samples was determined using an X-ray Diffractometer (XRD). The results revealed fluctuations in the size, lattice parameter, and strain in the nanoparticles with increasing the concentration of sodium acetate. Field-Emission Scanning Electron Microscopy (FESEM) was used to determine synthesized materials’ morphology and particle size. It revealed that the particles possessed approximately spherical morphology whose size decreased significantly with the increasing amount of sodium acetate. Transmission Electron Microscopy (TEM) was utilized to determine the structure, morphology, and elemental distributions in particles at the nanoscale, and it confirmed the findings of XRD and FESEM analyses. The high-resolution TEM (HRTEM) imaging analysis of the nanoparticles in our studied samples revealed that the particles predominantly possessed (001) type facets. X-ray photoelectron spectroscopy (XPS) and core-loss electron energy loss spectroscopy (EELS) showed an increasing fraction of Fe2+ with the decreasing size of the particles in samples. The Brunauer, Emmett, and Tellers (BET) analysis of samples revealed a higher surface area as the particle size decreases. In addition, the determined surface area and pore size values are compared with the literature, and it was found that the synthesized materials are promising for gas-sensing applications. The ab initio calculations of the Density of States (DOS) and Band structure of (001) surface terminating ZnFe2O4 were carried out using Quantum Espresso software to determine the bandgap of the synthesized samples. They were compared to their corresponding experimentally determined bandgap values and showed close agreement. Finally, in-situ TEM measurement was carried out on one of the four studied samples with robust properties using Ar and CO2 as reference and target gases, respectively. It is concluded from the presented study that the size reduction of the ZnFe2O4 nanoparticles (NPs) tunes the bandgap and provides more active sites due to a higher concentration of oxygen vacancies. The in-situ TEM showed us a nanoscale observation of the change in one of the crystal structure parameters. The d spacing of ZnFe2O4 NPs showed a noticeable fluctuation, reaching more than 5% upon exposure to CO2 and Ar gases.
Iron-doped titanium dioxide nanoparticles, with Fe/Ti atomic ratios from 0% to 10%, were synthesized by flame spray pyrolysis (FSP), employing a single-step method. Ferrocene, being nontoxic and readily soluble in liquid hydrocarbons, was used as the iron source, while titanium tetraisopropoxide (TTIP) was used as the precursor for TiO2. The general particle characterization and phase description were examined using ICP-OES, XRD, BET, and Raman spectroscopy, whereas the XPS technique was used to study the surface chemistry of the synthesized particles. For particle morphology, HRTEM with EELS and EDS analyses were used. Optical and magnetic properties were examined using UV–vis and SQUID, respectively. Iron doping to TiO2 nanoparticles promoted rutile phase formation, which was minor in the pure TiO2 particles. Iron-doped nanoparticles exhibited a uniform iron distribution within the particles. XPS and UV–vis results revealed that Fe2+ was dominant for lower iron content and Fe3+ was common for higher iron content and the iron-containing particles had a contracted band gap of ~1 eV lower than pure TiO2 particles with higher visible light absorption. SQUID results showed that doping TiO2 with Fe changed the material to be paramagnetic. The generated nanoparticles showed a catalytic effect for dye-degradation under visible light.
Natural or synthetic graphite as precursors for the preparation of graphene oxide (GO) have constraints due to their limited availability, high reaction temperature for processing of synthetic graphite and higher generation cost. The use of oxidants, long reaction duration, the generation of toxic gases and residues of inorganic salts, the degree of hazard and low yield are some of the disadvantages of the oxidative-exfoliation methods. Under these circumstances, biomass waste usage as a precursor is a viable alternative. The conversion of biomass into GO by the pyrolysis method is ecofriendly with diverse applications, which partially overcomes the waste disposal problem encountered by the existing methods. In this study, graphene oxide (GO) is prepared from dry leaves of sugarcane plant through a two-step pyrolysis method using ferric (III) citrate as a catalyst, followed by treatment with conc. H2SO4. The synthesized GO is analyzed by UV-Vis., FTIR, XRD, SEM, TEM, EDS and Raman spectroscopy. The synthesized GO has many oxygen-containing functional groups (–OH, C–OH, COOH, C–O). It shows a sheet-like structure with a crystalline size of 10.08 nm. The GO has a graphitic structure due to the Raman shift of G (1339 cm−1) and D (1591 cm−1) bands. The prepared GO has multilayers due to the ratio of 0.92 between ID and IG. The weight ratios between carbon and oxygen are examined by SEM-EDS and TEM-EDS and found to be 3.35 and 38.11. This study reveals that the conversion of sugarcane dry leaves into the high-value-added material GO becomes realistic and feasible and thus reduces the production cost of GO.