Layered double hydroxides (LDHs) are a class of anionic clays consisting of positivelycharged brucite-like layers between which are intercalated anions and water molecules. LDHs containing Mg2+ and Al3+ cations with molar ratio of 2.5 were prepared by co-precipitation. Intercalation of an organic chromophore in layered double hydroxide (LDH) materials was done by reconstruction method. Coumarin intercalated inside the interlayers, induce changes in their morphology and in optical properties. X-ray diffraction (XRD), FT-IR spectroscopy, thermogravimetric analysis and differential thermal analysis (TG-DTA) analysis on prepared powders shows that the coumarin-343 has been successfully intercalated into LDH matrix. The minimal amount of incorporated coumarin-343 is 1.1% and was determined by TG analysis. Thin films of coumarin intercalated in LDH structure have been prepared by pulsed laser deposition (PLD) using a Nd:YAG laser working at 532 nm and 1064 nm and 10 Hz repetition rate [1,2]. The optical properties of hybrid thin films were characterized by photoluminescence spectra with the excitation wavelength of 380 nm pumped by Xe lamp.