Curcumin (CR) is a natural compound with a well-known antioxidant and therapeutic activity. Its stability may be enhanced when incorporated in different matrices as a layered double hydroxides (LDH) matrix. Curcumin intercalated layered double hydroxide nanohybrid is a potential drug delivery system for effective photodynamic therapy in human breast cancer or skin cancer. The synthesis of the hybrid LDH-CR powder implies the dissolution of CR in water or in another organic solvent which is miscible with water. Since the solubility of curcumin in water is very weak, the aim of this study is to investigate the effect of the solvent employed for its dissolution on the structural and physico-chemicalphotoluminescent properties of the resulting hybrid materials. Four powders of curcumin (CR)-containing Mg2.5Al-LDH hybrids (Mg/Al molar ratio of 2.5) were prepared by co-precipitation (P) and reconstruction (R) using two different solvents for the dissolution of curcumin: (i) an alkaline aqueous solution (A), and (ii) ethanol (E). The reconstruction used the calcinated (460 degrees C for 18 h) form of the parent Mg2.5Al-LDH powder. All the solids were characterized by X-ray diffraction (XRD), and FTIR spectroscopy. The FTIR-ATR spectra of the all the powders except the powder prepared via reconstruction in ethanol exhibit LDH characteristics, consistent with the XRD results. Matrix Assisted Pulsed Laser Evaporation (MAPLE) was employed for the deposition of hybrid LDH-CR thin films. Aqueous solutions of the as prepared hybrid LDH-CR powders were frozen and used as targets for MAPLE depositions. The films were deposited using a nanosecond laser emitting at 266 nm. MAPLE is considered a "soft" deposition technique suitable to conserve the CR stability. XRD, scanning electron microscopy, FT-IR spectroscopy and fluorescence measurements were used to characterize the deposited films in order to evidence the influence of the preparation methods on the structural and photophysical characteristics of the hybrid LDH-CR films.