In recent years, electrocatalytic reduction of CO₂ has been a focus in the research field. There are also various methods for synthesizing catalysts, such as the hydrothermal method, the arc method, electrospinning, etc. Here, we introduce the electrochemical deposition method. Compared with ordinary synthesis methods, electrodeposition has the advantages of simple processing, controllable conditions, high safety, and environmental friendliness. It is also a promising method for industrialized catalyst synthesis. In this review, we give a detailed introduction to electrodeposition, summarize the research progress of electrodeposition in the synthesis of catalysts, and discuss the key conditions in the preparation process, which are provided as a reference to synthesize next-generation electrodeposited electrocatalysts.

Noble metal catalysts have extraordinary catalytic activity but suffer from high cost; therefore single atom catalysis attracts tremendous attention. Here, we propose atom-scale dispersed palladium (Pd) in a layered TaS₂ lattice to form new compounds of Pd_xTaS₂, whose crystal structure was resolved by powder X-ray diffraction. The electrical conductivity of metallic Pd_0.1TaS₂ (1.36 × 10⁴ S m⁻¹) is twice as large as that of TaS₂ (6.18 × 10³ S m⁻¹). This compound applied as a new electrocatalyst for the hydrogen evolution reaction (HER) exhibits excellent catalytic performance with an onset overpotential of 77 mV, superior to those of other catalysts such as TaS₂ (295 mV) and Pd-loaded TaS₂ (114 mV). Density functional theory calculations reveal that the interaction of Pd-4d and Ta-5d orbitals results in the upshift of the Fermi level (TaS₂versus Pd_0.1TaS₂) to decrease the barrier height for the HER. Furthermore, the hybridization of Pd-4d and S-3p orbitals builds up pathways along the c axis to improve the conductivity and promote HER performance. It is noted that the amount of Pd used in Pd_0.1TaS₂ is only 4 wt%, compared with 20 wt% in commercial Pd/C catalysts, which is beneficial for its practical application.

Electrochemical conversion of CO₂ (CO₂RR) into high-value fuel is identified as one of the promising approaches to achieve carbon neutrality. The synthesis of high-efficiency CO₂ reduction electrocatalysts with high C₂:C₁, selectivity remains a field of intense interest. Previous studies have shown that the presence of Cu(I) is beneficial for the reduction of CO₂ into C₂ products. However, the stable presence of Cu(I) remains controversial, especially in the negative potential window. Here we report a simple and easily scalable catalyst precursor Cu₂(OH)₃Cl/C, which automatically forms in-situ chlorine-doped Cu/Cu₂O heterointerface during electrocatalysis. The catalyst not only exhibits a Faradaic efficiency of 33.03% but also provides a long-term stability of Cu⁺, gaining a stable electrolysis of 11 h, with an ethylene/methane ratio over 50. The experimental results and mechanistic studies confirm that the presence of Cl⁻ inhibits the reduction of Cu⁺, inducing the formation of Cu⁰/Cu⁺, and reduces the reaction energy of the intermediate ⋆CO dimerization, thereby facilitating the formation of C₂ products. This work provides a feasible way to synthesize copper ions with long-term and stable positive charge in CO₂RR and expands a new way to synthesize ethylene industrial products in the future.