The design of catalysts with high activity, selectivity, and stability is key to the electroreduction of CO2. Herein, we report the synthesis of 3D hierarchical metal/polymer–carbon paper (M/polymer‐CP) electrodes by in situ electrosynthesis. The 3D polymer layer on CP (polymer‐CP) was first prepared by in situ electropolymerization, then a 3D metal layer was decorated on the polymer‐CP to produce the M/polymer‐CP electrode. Electrodes with different metals (e.g. Cu, Pd, Zn, Sn) and various polymers could be prepared by this method. The electrodes could efficiently reduce CO2 to desired products, such as C2H4, CO, and HCOOH, depending on the metal used. For example, C2H4 could be formed with a Faradaic efficiency of 59.4 % and a current density of 30.2 mA cm−2 by using a very stable Cu/PANI‐CP electrode in an H‐type cell. Control experiments and theoretical calculations showed that the 3D hierarchical structure of the metals and in situ formation of the electrodes are critical for the excellent performance.

We have synthesized NbOx with oxygen vacancies (OVs) and conducted the first work for nitrate electroreduction to NH3 over Nb oxides. It was a robust non-precious metal catalyst for NH3...

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ILs with an azobenzene-group at the end of the alkyl chain could form micelles; UV/vis irradiation only changed the size of the aggregates.

The rich oxygen vacancies in Bi2WO6 nanosheets can efficiently enhance CO2 electroreduction to CO.