Development of the Sb4O5Cl2@NbSe2 Composite: The Impact of 2H-NbSe2 Nanoparticles on Sb4O5Cl2 and Their Application for the Removal of Cr(VI)/Fe(III) and Methyl Orange from Wastewater.

A potential adsorbent, Sb4O5Cl2@NbSe2 composite, was generated from the Sb4O5Cl2 photocatalyst and 5 wt % layered 2H-NbSe2 nanoparticles for the highly effective removal of Cr(VI) and Fe(III) ions and methyl orange (MO) from aqueous solution, and a comparison was drawn against the precursors. Sb4O5Cl2 crystallites and NbSe2 nanoparticles were synthesized hydrothermally, and the composite was prepared by the incipient wetness impregnation technique. The crystal structure of Sb4O5Cl2 was determined by single-crystal X-ray diffraction (SCXRD) data. Powder X-ray diffraction (PXRD) study revealed the 2H phase of NbSe2 nanoparticles. Field emission scanning electron microscopy (FESEM) analysis confirmed the formation of the spherical-shaped NbSe2 nanoparticles from rod-shaped bulk 2H-NbSe2. Morphological changes from the hexagonal to irregular prismatic shape were found upon the formation of the Sb4O5Cl2@NbSe2 composite compared to pure Sb4O5Cl2. Negative ζ-potential values indicated that electrostatic interactions were the predominant factor for the adsorption process. Sb4O5Cl2@NbSe2 provided removal efficiencies of 99% for MO in 6 h, 96.52% for Cr(VI) within 2.5 h, and 92.43% for Fe(III) within 4 h of 10 mg/L initial concentration. The maximum adsorption capacities of the composite for MO, Fe(III), and Cr(VI) were found to be 66.56, 131.48, and 122.30 mg/g, respectively, as calculated using the Langmuir isotherm equation.

CuAs2O4: Design, Hydrothermal Synthesis, Crystal Structure, Photocatalytic Dye Degradation, Hydrogen Evolution Reaction, Knoevenagel Condensation Reaction, and Thermal Studies.

CuAs2O4 has been explored as a heterogeneous catalyst in the fields of photocatalysis, electrocatalysis, and solvent-free organic transformation reactions. The homogeneity has been successfully attained for the first time by designing a pH-assisted hydrothermal synthesis technique. Single-crystal X-ray diffraction studies reveal that no phase transition has been observed by lowering the temperature up to 103 K with no existence of satellite reflections. The crystal structure exhibits tetragonal symmetry with space group P42/mbc and consists of [CuO6] octahedra and [AsO3E] tetrahedra (E represents the stereochemically active lone pair). Structural investigation shows a cylindrical void inside the structure, which could lead to interesting physical and chemical properties. The photocatalytic dye degradation efficiency with methylene blue (MB) showed ∼100% degradation, though the degradation efficiency increased by 2-fold with the addition of 6% H2O2. The reusability of the catalyst up to the 10th cycle with ∼35% MB dye degradation has been established. It can exhibit HER activity with a low overpotential of 165 mV with respect to RHE to attain the current density of j = 10 mA cm-2. SEM and TEM revealed rod-shaped particles, which supported the large number of catalytic active sites. The structural consistency of the catalyst after photodegradation and HER studies is confirmed by the PXRD pattern. XPS confirms the oxidation state of Cu and As in the compound. The catalytic activity toward the Knoevenagel condensation reaction at moderate temperature under solvent-free condition is also studied. TG-DTA shows an endothermic minimum (Tmin) at 436 °C due to the mass loss of As2O3.

Zn3Sb4O6F6 and KI-Doped Zn3Sb4O6F6: A Metal Oxyfluoride System for Photocatalytic Activity, Knoevenagel Condensation, and Bacterial Disinfection.

Zn3Sb4O6F6 crystallites were synthesized by a pH-regulated hydrothermal synthetic approach, while doping on Zn3Sb4O6F6 by KI was performed by the "incipient wetness impregnation technique." The effect of KI in Zn3Sb4O6F6 is found with the changes in morphology in the doped compound, i.e., needle-shaped particles with respect to the irregular cuboid and granular shaped in the pure compound. Closer inspection of the powder diffraction pattern of doped compounds also reveals the shifting of Braggs' peaks toward a lower angle and the difference in cell parameters compared to the pure compound. Both metal oxyfluoride comprising lone pair elements and their doped compounds have been successfully applied as photocatalysts for methylene blue dye degradation. Knoevenagel condensation reactions were performed using Zn3Sb4O6F6 as the catalyst and confirmed 99% yield even at 60 °C temperature under solvent-free conditions. Both pure and KI-doped compounds were tested against several standard bacterial strains, i.e., Enterobacter sp., Escherichia coli, Staphylococcus sp., Salmonella sp., Bacillus sp., Proteous sp., Pseudomonas sp., and Klebsiella sp. by the "disk diffusion method" and their antimicrobial activities were confirmed.

pH-regulated hydrothermal synthesis and characterization of Sb4O5X2 (X = Br/Cl) and its use for the dye degradation of methyl orange both with and without light illumination.

A pH-regulated hydrothermal synthesis method was employed to synthesize Sb4O5Br2 and Sb4O5Cl2 crystallites. Characterization is done by single crystal X-ray diffraction, powder X-ray diffraction, infra-red spectroscopy, scanning electron microscopy and DFT studies. The compounds crystallize in monoclinic symmetry with a P21/c space group. Complete structural analysis of the Sb4O5Br2 compound by using single crystal X-ray diffraction data is performed for the first time and a comparative study with Sb4O5Cl2 is also discussed. The SEM study reveals that the surface morphology changes with the variation of pH for bromide compounds, whereas pH change does not affect the morphology of the chloride analogues. Electronic band structures of the synthesized oxyhalides were investigated in order to understand their catalytic effects in the dye degradation reactions in dark as well as sunlight conditions.