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So far no reports have been seen on the spectroscopic studies of CuO-doped monoliths heated at different temperatures. The present work aims at understanding the effect of thermal treatment on the spectroscopic properties of different copper concentrations (2, 5, and 10 wt. %). The characterization of the xerogel samples was done by Uv-vis, FTIR, Raman spectroscopy and TEM micrographic at different temperatures. In a recent investigation, host matrices were extensively embedded with copper oxide that was produced with one distinct concentration of about (2-10 wt. %). The characterization of xerogel was done by thermal gravimetric analysis (TGA), X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), surface analysis (such as; BET) and thermal-program reduction (TPR) methods at different temperatures. The recent investigation was devoted to the systematic reactivity study of N2O decomposition on dispersed copper oxide nano-catalysts over silica supports, in order to determine the ability of these materials to convert di-nitrogen oxide into harmless species by different temperatures. The host matrices were extensively embedde