Urea electrosynthesis under mild conditions shows great potential to conquer the conventional manufacturing industry with huge energy consumption. Here, self-supported oxygen vacancy-rich ZnO (ZnO-V) porous nanosheets are prepared using the electroreduction method and adopted as an efficient catalyst for aqueous urea electrosynthesis by using CO₂ and nitrite contaminants as feedstocks. The urea Faradaic efficiency of ZnO-V achieves 23.26% at −0.79 V versus the reversible hydrogen electrode (RHE), which is almost 3 times as high as that of ZnO (8.10%). Liquid chromatography is developed for quantitative analysis of urea. The combined results of online differential electrochemical mass spectrometry (DEMS) and in situ diffuse reflectance infrared Fourier transform spectroscopy unveil a possible coupling pathway of NH₂∗ and COOH∗ intermediates for urea formation. Our work opens an avenue for rational construction of efficient electrocatalysts for urea electrosynthesis and broadens the scope of products available from nitrite and CO₂ reduction.

在温和条件下进行尿素电合成显示出巨大的潜力，以巨大的能耗来征服常规制造业。在此，使用电还原方法制备自支撑的富氧空位的ZnO（ZnO-V）多孔纳米片，并通过使用CO ₂和亚硝酸盐污染物作为原料，将其用作尿素电合成的有效催化剂。与可逆氢电极（RHE）相比，ZnO-V的尿素法拉第效率在-0.79 V时达到23.26％，几乎是ZnO（8.10％）的三倍。开发了液相色谱法用于尿素的定量分析。在线差分电化学质谱（DEMS）和原位分析的综合结果漫反射红外傅里叶变换光谱揭示了NH ₂＊和COOH ＊中间体形成尿素的可能耦合途径。我们的工作为合理构建尿素电合成的高效电催化剂开辟了道路，并拓宽了亚硝酸盐和CO ₂还原产品的适用范围。