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As atmospheric CO2 concentrations continue to rise rapidly in response to increased combustion of fossil fuels, the development of robust adsorbents for the selective capture of CO2 from the flue gas stream of fossil-fired power plants appears critically important from the perspective of climate change mitigation. Attributing to their enormous specific surface area, intense porosity, physically linked permeable networks and high-class sturdiness among others, three-dimensional (3D) graphene-based macromolecular assemblies (GMAs) hold significant promise for CO2 adsorption and separation applications. The current chapter outlines the recent advancements toward the exploration of 3D GMAs as a new class of adsorbent for postcombustion carbon capture. In addition, the numerous surface modification schemes that are actively pursued to enrich the CO2 adsorption capacity of 3D GMAs are comprehensively examined. Finally, associated challenges are pointed out and strategic research guidelines are proposed, with an eye on the foreseeable future.

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