Visible light-active nickel-based plasmonic photocatalysts provide a cost-effective alternative to noble metals. However, their rarity, fragility, and limited understanding pose challenges. This work presents a microwave-assisted organic synthesis of a Ni-NiO@Ni2CO3(OH)2 core-shell@sheet plasmonic photocatalyst. By employing time and power dependent synthesis, this catalyst exhibits flexible Ni2CO3(OH)2 nanosheets enveloping the Ni-NiO structure, surpassing the pristine Ni@NiO/NiCO3 core-shell counterpart. Chemical reaction mechanisms suggest that irradiation of pristine Ni-NiO/NiCO3 nano structures leads to breakage of amorphous NiCO3 to Ni2+ and CO32-, which further, in the presence of water solvent, interacts with OH- ions leading to the formation of Ni(CO3)·Ni(OH)2. With enhanced light absorption and photocatalytic properties, the resulting core-shell@sheet photocatalyst demonstrates double the hydrogen evolution reaction yield (40 μmol g-1 h-1) compared to the pristine catalyst (20 μmol g-1 h-1). The enhanced H2 yield is attributed to the flexible sheets, cross-dimensional photocatalyst structure, increased surface area for surface reactions, and higher H2 activity of Ni2CO3(OH)2. This research showcases the potential of microwave-assisted synthesis in developing flexible nanosheets with superior solar water splitting performance.
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