隨著全球暖化與氣候危機加劇，工業化所造成的碳排放與含氮廢水污染已成為亟待解決的環境議題。二氧化碳還原反應（CO2RR）可將CO2轉化為甲酸等高附加價值產物，而硝酸根還原反應（NO3RR）則能將廢水中的硝酸根轉化為氨等重要化學品。本研究整合CO2RR與NO3RR，透過共電解策略實現尿素之電化學合成。尿素是重要農業肥料與工業原料，然而，傳統尿素製程伴隨大量能源消耗，因此開發低能耗且高效率的電化學尿素合成技術，對於推動永續化學品製造具有重要意義。 本研究以簡易熱處理方式對泡沫銅（copper foam， CF）進行表面改質，透過依序硒化、硫化並引入TiO2修飾，成功製備CuSe-S-TiO2/CF自支撐觸媒。該觸媒在-0.05 V vs. RHE下尿素法拉第效率達55%，相較於CuSe-S/CF提升超過三倍，並較CuSe/CF提升超過十倍。此外，CuSe-S-TiO2/CF在連續反應20小時後仍維持高效率尿素產出，顯示優異長時間穩定性。 X光繞射(XRD)與非原位拉曼光譜(Ex-situ Raman spectrum)結果顯示，CuSe-S-TiO2/CF 具有較高比例之Cu2O相，有效提升催化活性與反應中間體吸附能力。原位拉曼光譜(In-situ Raman spectrum)進一步證實，其反應過程中產生明顯*CO2NH2中間體與C-N鍵振動訊號，顯示該觸媒可有效促進碳氮偶聯反應。綜上所述，本研究提出具高效率與高穩定性之尿素共電解觸媒，為碳排放與含氮廢水資源化提供具潛力之永續策略。;With the intensification of global warming and the climate crisis， carbon emissions and nitrogen-containing wastewater from industrialization have become urgent environmental issues. The carbon dioxide reduction reaction (CO2RR) can convert CO2 into value-added products such as formate， while the nitrate reduction reaction (NO3RR) can transform nitrate in wastewater into important chemicals such as ammonia. In this study， CO2RR and NO3RR were integrated through a co-electrolysis strategy for electrochemical urea synthesis. As urea is an important agricultural fertilizer and industrial feedstock， developing a low-energy and efficient electrochemical route is significant for sustainable chemical production. A facile thermal treatment method was used to modify copper foam (CF) through sequential selenization， sulfurization， and TiO2 modification， producing a self-supported CuSe-S-TiO2/CF catalyst. The catalyst achieved a urea Faradaic efficiency of 55% at -0.05 V vs. RHE， which was more than three times higher than that of CuSe-S/CF and over ten times higher than that of CuSe/CF. It also maintained efficient urea production after 20 h of continuous electrolysis， demonstrating excellent long-term stability. X-ray diffraction (XRD) and ex-situ Raman spectroscopy showed that CuSe-S-TiO2/CF contained a higher proportion of Cu2O signals， effectively enhancing catalytic activity and intermediate adsorption. In-situ Raman spectroscopy further confirmed the formation of *CO2NH2 intermediates and C-N bond vibration signals， indicating efficient carbon-nitrogen coupling. Overall， this study presents a highly efficient and stable co-electrolysis catalyst for urea synthesis， offering a promising strategy for valorizing carbon emissions and nitrogen-containing wastewater.
