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The electrocatalytic reduction of CO2 to high value‐added chemicals is one of the effective technologies to achieve the goal of carbon neutralization. However, highly selective production of hydrocarbon via electrochemical conversion of CO2 still has great challenges. Herein, a unique CuO phase composition is constructed that consists of rectangular nanoflakes possessing crystalline/amorphous structures by the facile strategy. Crystalline CuO square nanoblocks are confined in amorphous nanoflakes and form crystalline/amorphous hybrid phase. The results of electrocatalytic CO2 reduction demonstrate that this crystalline/amorphous CuO material exhibits superior CO2 conversion ability with ethylene Faradaic efficiency of 58.3 % at −1.08 V vs. RHE, which is ascribed to nanoflake structures and fast electron transfer on the crystalline/amorphous interfaces because of superior conductivity of amorphous CuO. The present research provides an effective route to reconstruct novel crystalline/amorphous interfaces of CuO for catalysis applications. [ABSTRACT FROM AUTHOR]

Electrochemical water splitting has been considered as a promising method for large‐scale hydrogen production. However, the development of high‐performance and low‐cost noble metal‐free electrocatalysts for hydrogen evolution reaction (HER) remains a great challenge. Transition metal carbides (such as molybdenum carbide) are one of the most potential substitutes for noble metal as electrocatalysts for HER. One of the effective measures for further enhancing their performances is to hinder the coalescence of nanoparticles. Here we demonstrate a two‐dimensional ultrafine molybdenum carbide‐coupled mesoporous structured meshlike carbon nanolayers synthesized vis facile route based on holes in the carbon nanolayer structures blocking nanoparticle agglomeration. Molybdenum carbide clusters dispersed on the carbon nanolayers are successfully prepared by carbonization of molybdate‐polyvinylpyrrolidone precursor as a proof of concept, which exhibits excellent electrocatalytic activity for the HER and high stability in basic medium. The present study provides some references for the design and synthesis of nanostructured electrocatalysts utilizing 2D meshlike materials to prevent nanoparticles from agglomerating. [ABSTRACT FROM AUTHOR]