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The development of bifunctional electrocatalysts that are reliable, stable, and affordable for overall water splitting reactions (OWSs) has evolved into a top priority, considering the urgent need to promote sustainable energy-based green hydrogen generation technologies. Because of the advantages associated with their special 2D layer arrangement and remarkable physical and chemical features, layered double hydroxides (LDHs) containing transition metal ions have attracted extensive research attention and are considered as bifunctional electrocatalysts with the greatest potential. This chapter provides an overview of the most recent cutting-edge approaches to the development of LDHs, such as anion intercalation, defect engineering, cation doping, preparing the hierarchical heterostructure, and the formation of LDH derivatives. The function of these LDHs in OWSs, the way in which transition metal-based catalysts can maintain the hydrogen evolution reaction/oxygen evolution reaction (HER/OER), and the reaction mechanisms are all highlighted in this chapter.

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