Solar energy is one of the elements that have been used as a resource in the green energy field. Hydrogen, as an energy carrier, can be produced from many kinds of sources, including solar energy. Here, we present two-dimensional (2D)perovskite material derived from the Dion-Jacobson phase (DJ), Ca2Nan-3NbnO3n+1- (CNNO−) nanosheets, with the number of layer n = 4–6 synthesized via microwave-assisted hydrothermal method. The starting material KCa2Nb3O10 (KCNO) is made from two methods. The solid-state calcination KCNO product has more than two-phase, while the molten-salt synthesis produces a well cubic KCNO crystalline. TThe thickness of the 2D CNNO− nanosheets is increasing, in dependence on the n value. Meanwhile, the estimated optical band gap is decreasing, in dependence on the n value. 2D CNNO− nanosheets show the absorbance under ultraviolet (UV) light, which confirms their semiconducting nature. The capability of these 2D nanosheets to generate hydrogen is presented via photo-electrochemical (PEC) water splitting. The molten-salt fabricated CNNO− nanosheets CNNO6 shows better performance with the highest efficiency ɳ up to 0.110% when applied to the PEC device.
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