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Two-dimensional (2D) nanostructured materials are emerging catalysts for different electrochemical reactions, including water splitting reaction, nitrogen reduction reaction (N2RR), and CO2 electrochemical reduction reaction (CO2RR). This chapter presents the essential fundamental properties of 2D nanostructured materials, and their performances for CO2RR in terms of product selectivity, catalytic activity, and CO2RR mechanism. A number of 2D nanomaterials such as graphene, metal nanosheets, metal oxides, transition metal dichalcogenides (TMDCs), metal–organic framework thin films, and hybrids compositions are highlighted as a state-of-the-art catalysts towards CO2RR. This chapter also includes further discussion on different pathways for engineering 2D materials for CO2RR. Next, the configurations, operating principles and key advantages/disadvantages of different types of electrolyzer used to study CO2RR are discussed. Finally, challenges and future directions associated with the role of 2D nanocatalysts and electrolyzers for the scale-up of CO2RR are discussed.

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