Nano-hybrid promoted as materials with improved optical properties. The aim of this study was to analyze differences in optical properties at micro-scale. This research focuses on the impact of reaction temperature during the creation of magnesium nitrate-tricine nanoparticles through chemical vapor deposition. The study investigates how temperatures of 200°C and 300°C affect the particle size, crystallinity, and morphology of the nanoparticles. Optimizing these properties is essential for achieving the desired third-order NLO effect. By understanding the influence of temperature on nanoparticle characteristics, researchers can develop more effective NLO materials for future photonic devices. This study explores the chemical and structural differences between MNT 300 and MNT 400 materials using various techniques. Spectroscopic analysis reveals similarities in both materials with a shared peak at 1400 cm−1. However, MNT 400 exhibits additional peaks suggesting the presence of aromatic rings, nitro compounds, or variations in N–H bonds. Both MNT 300 and MNT 400 exhibit micro porous behaviour with a narrow pore size distribution around 14 nm to 15 nm, indicating tightly packed structures. Transmission Electron Microscopy analysis shows a wide particle size range (2 nm to 200 nm) in both materials, suggesting the presence of atomic clusters, individual molecules, and potentially agglomerated structures. FT-Raman spectroscopy reveals higher intensity peaks in MNT 400, which could be due to a higher concentration of specific bonds, a more ordered structure, or enhanced Raman scattering. This suggests greater crystallinity or molecular uniformity in MNT 400 compared to MNT 300.