Photocatalytic CO2 reduction attracts substantial interests for the production of chemical fuels via solar energy conversion, but the activity, stability, and selectivity of products were severely determined by the efficiencies of light harvesting, charge migration, and surface reactions. Structural engineering is a promising tactic to address the aforementioned crucial factors for boosting CO2 photoreduction. Herein, a timely and comprehensive review focusing on the recent advances in photocatalytic CO2 conversion based on the design strategies over nano‐/microstructure, crystalline and band structure, surface structure and interface structure is provided, which covers both the thermodynamic and kinetic challenges in CO2 photoreduction process. The key parameters essential for tailoring the size, morphology, porosity, bandgap, surface, or interfacial properties of photocatalysts are emphasized toward the efficient and selective conversion of CO2 into valuable chemicals. New trends and strategies in the structural design to meet the demands for prominent CO2 photoreduction activity are also introduced. It is expected to furnish a comprehensive guideline for inside‐and‐out design of state‐of‐the‐art photocatalysts with well‐defined structures for CO2 conversion.

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Monolayered photocatalytic materials have attracted huge research interests in terms of their large specific surface area and ample active sites. Sillén-structured layered BiOX (X = Cl, Br, I) casts great prospects owing to their strong photo-oxidation ability and high stability. Fabrication of monolayered BiOX by a facile, low-cost, and scalable approach is highly challenging and anticipated. Herein, we describe the large-scale preparation of monolayered BiOBr nanosheets with a thickness of ∼0.85 nm via a readily achievable liquid-phase exfoliation strategy with assistance of formamide at ambient conditions. The as-obtained monolayered BiOBr nanosheets are allowed diverse superiorities, such as enhanced specific surface area, promoted band structure, and strengthened charge separation. Profiting from these benefits, the advanced BiOBr monolayers not only show excellent adsorption and photodegradation performance for treating contaminants, but also demonstrate a greatly promoted photocatalytic activity for CO2 reduction into CO and CH4. Additionally, monolayered BiOI nanosheets have also been obtained by the same synthetic approach. Our work offers a mild and general approach for preparation of monolayered BiOX, and may have huge potential to be extended to the synthesis of other single-layer two-dimensional materials.

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Layered BiIO4/Bi2WO6 (2, 5, 10, and 15%) heterojunctions are prepared by hydrothermal processing of an aqueous suspension of Bi(NO3)3 and a I2O3, Na2WO4 solution (autoclave, 180 °C, 1 d).