ABSTRACTThis study presents a green approach for urea synthesis using plasma–ice interaction with N₂ + CO₂ and NH₃ + CO₂ gas mixtures. Plasma characterization via electrical and optical emission spectroscopy revealed that urea formation involves complex reactions driven by high‐energy species, producing reactive nitrogen and carbon intermediates. Plasma‐treated ice exhibited increased pH, electrical conductivity (EC), and reduced oxidation–reduction potential (ORP). Optimization of parameters, especially treatment time, significantly influenced urea formation. The NH₃ + CO₂ plasma produced a higher urea concentration (7.7 mg L−1) compared to the N₂ + CO₂ plasma (0.55 mg L−1) due to ammonia's greater reactivity. This method offers a sustainable, energy‐efficient alternative to traditional urea synthesis processes.