A mixed crystal of urea–thiourea was grown by slow evaporation of aqueous solution at room temperature. The bright and transparent crystals obtained were characterized by thermogravimetric–differential thermal analysis (TG–DTA), UV and FTIR spectroscopic analyses. A fitting decomposition pattern for the title compound was formulated on the TG curve which shows a two stage weight loss between 200 and 750 °C. In this temperature range DTA curve shows exothermic peaks supporting the formulated decomposition pattern. The UV and FTIR spectra show the characteristic absorption, vibration frequencies due to urea–thiourea mixed crystals. Detailed structural analysis of the compound is under progress.