Exfoliated graphitic carbon nitride (ex-g-CN) was synthesized and loaded with non-noble metals (Ni, Cu, and Co). The synthesized catalysts were tested for hydrogen production using a 300-W Xe lamp equipped with a 395 nm cutoff filter. A noncommercial double-walled quartz-glass reactor irradiated from the side was used with a 1 g/L catalyst in 20 mL of a 10 vol% triethanolamine aqueous solution. For preliminary screening, the metal-loaded ex-g-CN was synthesized using the incipient wetness impregnation method. The highest hydrogen production was observed on the Ni-loaded ex-g-CN, which was selected to assess the impact of the synthesis method on hydrogen production. Ni-loaded ex-g-CN was synthesized using different synthesis methods: incipient wetness impregnation, colloidal deposition, and precipitation deposition. The catalysts were characterized by X-ray powder diffraction, X-ray photoelectron spectroscopy, nitrogen adsorption using the Brunauer-Emmett-Teller method, and transmission electron microscopy. The Ni-loaded ex-g-CN synthesized using the colloidal method performed best with a hydrogen production rate of 43.6 µmol h-1 g-1. By contrast, the catalysts synthesized using the impregnation and precipitation methods were less active, with 28.2 and 10.1 µmol h-1 g-1, respectively. The hydrogen production performance of the suspended catalyst (440 µmol m-2 g-1) showed to be superior to that of the corresponding immobilized catalyst (236 µmol m-2 g-1).
Keywords: cocatalyst deposition; graphitic carbon nitride; hydrogen production; nickel; water splitting.