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Graphitic carbon nitride (g-C 3 N 4) modified with bromine and iodine was synthesized by a novel two-stage technique that included hydrothermal pre-treatment of melamine and its calcination in a mixture with ammonium halide. Prepared photocatalysts were tested by a set of methods including X-ray diffraction (XRD), diffuse reflectance spectroscopy (DRS), thermal gravimetric analysis (TGA), low temperature nitrogen adsorption, transmission electron microscopy (TEM), scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), cyclic voltammetry (CVA), impedance spectroscopy, and the Mott – Schottky method. All the photocatalysts were studied in the photocatalytic hydrogen production from triethanolamine (TEOA) under visible light irradiation (λ = 428 nm). The most active photocatalyst was prepared from a mixture of 50% NH 4 I and 50% melamine. Its catalytic activity (2120 μmol g−1 h−1) was 35 times higher than that of the catalyst synthesized by the simple calcination of melamine. The highest short-circuit current density of 2.7 mA/cm2 was obtained with a sample synthesized from the mixture of 80% NH 4 Br and 20% melamine. [Display omitted] • Halide-modified g-C 3 N 4 was prepared by a novel two-stage technique. • High catalytic activity was assigned to changes in S BET and electronic structure. • I-doped samples were more active in H 2 production than Br-doped ones. • The highest catalytic activity was 2120 μmol Н 2 g−1 h−1. • Br-doped samples demonstrated higher J sc than I-doped samples. [ABSTRACT FROM AUTHOR]

Novel composite photocatalysts consisting of a cadmium and zinc sulfide solid solution (Cd 0.6 Zn 0.4 S) and zinc sulfide (ZnS) nanoparticles were successfully prepared by a simple hydrothermal treatment of suspended Cd 0.3 Zn 0.7 S at 120 °C. The as-obtained materials were characterized by X-ray diffraction, X-ray photoelectron spectroscopy, and UV-VIS diffuse reflection spectroscopy. The obtained photocatalysts were tested in the photocatalytic evolution of hydrogen from a Na 2 S/Na 2 SO 3 aqueous solution under visible light irradiation (λ = 450 nm). It is shown that the hydrothermal treatment of Cd 0.3 Zn 0.7 S at 120 °C increases the activity by a factor of 7.5 due to the phase transformations of the solid solution with the formation of the multiphase Cd 0.6 Zn 0.4 S/ZnS sample. The deposition of gold on the surface of Cd 0.6 Zn 0.4 S/ZnS leads to a further increase in activity: the achieved photocatalytic activity and quantum efficiency (450 nm) for 1%Au/Cd 0.6 Zn 0.4 S/ZnS are 17.4 mmol g−1 h−1 and 42.6%, respectively. This excellent performance is found to be attributable to the transformation of Cd 1-x Zn x S from the cubic to the hexagonal phase during the hydrothermal treatment. Additionally, photoelectrodes based on Cd 0.6 Zn 0.4 S/ZnS and FTO were synthesized and tested in a two-electrode cell. A high value of the photocurrent equal to 0.5 mA/cm2 is achieved for the Cd 0.6 Zn 0.4 S/ZnS/FTO electrode. An investigation by means of impedance spectroscopy reveals the longer lifetime of photogenerated charge carriers in the Cd 0.6 Zn 0.4 S/ZnS/FTO photoelectrode if to compare with Cd 0.3 Zn 0.7 S/FTO system. Image 1 • Au/Cd 0.6 Zn 0.4 S/ZnS photocatalysts were prepared via simple hydrothermal synthesis. • The highest value of the photocatalytic activity was 17.4 mmol H 2 per hour per gram. • The highest apparent quantum efficiency was 42.6% (450 nm). • Photocurrent 0.5 mA/cm2 was achieved for the Cd 0.6 Zn 0.4 S/ZnS/FTO electrode. [ABSTRACT FROM AUTHOR]