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A key target to boost solar‐to‐chemical conversion processes is to fabricate an efficient solar‐light‐responsive photocatalyst. Herein, we report the in situ synthesis of nanoparticles (NPs) of Bi2O3 directly on Zn‐based layered double hydroxide (LDHs) frameworks. The in situ synthesis of Bi2O3NPs is done at room temperature, is ligand free and explores the ability of calcined ZnMeLDHs to reconstruct their layered structures in Bi(NO3)3 aqueous solution. The in situ formation of Bi2O3NPs on ZnMeLDHs is assessed by transmission electron microscopy (TEM), X‐ray photoelectron spectroscopy (XPS), powder X‐ray diffraction (XRD), and UV/Vis spectroscopy and compared with the features of a corresponding Bi2O3NPs/LDH prepared by the conventional impregnation route. The rapid photocatalytic response of the Bi2O3NPs/ZnMeLDH (Me=Al, Cr) heterostructures is confirmed by O2 generation from water under solar‐light irradiation. The rate of O2 generation increases by a factor of approximately 2 for the ZnCrLDH based catalysts as compared to that of the family of ZnAlLDH catalysts. Further, the presence of the bismuth phase and its nano‐dimension leads to increased efficiency for the in situ prepared Bi2O3NPs/LDHs as compared to that of impregnated Bi2O3/LDH and the pristine LDHs.

Artificially designed heterostructures formed by close conjunctions of plasmonic metal nanoparticles (PNPs) and non-plasmonic (2D) lamellar nanostructures are receiving extensive interest. The synergistic interactions of the nanounits induce the manifestation of localized surface plasmon resonance (LSPR) in plasmonic metals in the specific environment of the 2D-light absorbing matrix, impacting their potential in plasmon enhanced catalysis. Specifically, layered double hydroxides (LDH) with the advantages of their unique 2D-layered structure, tuned optical absorption, ease of preparation, composition diversity, and high surface area, have emerged as very promising candidates for obtaining versatile and robust catalysts. In this review, we cover the available PNPs/LDH heterostructures, from the most used noble-metals plasmonic of Au and Ag to the novel non-noble-metals plasmonic of Cu and Ni, mainly focusing on their synthesis strategies toward establishing a synergistic response in the coupled nanounits and relevant applications in plasmonic catalysis. First, the structure–properties relationship in LDH, establishing the desirable features of the 2D-layered matrix facilitating photocatalysis, is shortly described. Then, we address the recent research interests toward fabrication strategies for PNPs/support heterostructures as plasmonic catalysts. Next, we highlight the synthesis strategies for available PNPs/LDH heterostructures, how these are entangled with characteristics that enable the manifestation of the plasmon-induced charge separation effect (PICS), co-catalytic effect, or nanoantenna effect in plasmonic catalysis with applications in energy related and environmental photocatalysis. Finally, some perspectives on the challenges and future directions of PNPs/LDHs heterostructures to improve their performance as plasmonic catalysts are discussed.

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