Synthesis of Sulfur@g-C 3 N 4 and CuS@g-C 3 N 4 Catalysts for Hydrogen Production from Sodium Borohydride.

In this work, the S@g-C 3 N 4 and CuS@g-C 3 N 4 catalysts were prepared via the polycondensation process. The structural properties of these samples were completed on XRD, FTIR and ESEM techniques. The XRD pattern of S@g-C 3 N 4 presents a sharp peak at 27.2° and a weak peak at 13.01° and the reflections of CuS belong to the hexagonal phase. The interplanar distance decreased from 0.328 to 0.319 nm that facilitate charge carrier separation and promoting H 2 generation. FTIR data revealed the structural change according to absorption bands of g-C 3 N 4 . ESEM images of S@g-C 3 N 4 exhibited the described layered sheet structure for g-C 3 N 4 materials and CuS@g-C 3 N 4 demonstrated that the sheet materials were fragmented throughout the growth process. The data of BET revealed a higher surface area (55 m 2 /g) for the CuS-g-C 3 N 4 nanosheet. The UV-vis absorption spectrum of S@g-C 3 N 4 showed a strong peak at 322 nm, which weakened after the growth of CuS at g-C 3 N 4 . The PL emission data showed a peak at 441 nm, which correlated with electron-hole pair recombination. The data of hydrogen evolution showed improved performance for the CuS@g-C 3 N 4 catalyst (5227 mL/g·min). Moreover, the activation energy was determined for S@g-C 3 N 4 and CuS@g-C 3 N 4 , which showed a lowering from 47.33 ± 0.02 to 41.15 ± 0.02 KJ/mol.