In this paper, unique nanocomposites of Gold: Lithium Niobate (Au-LiNbO3) were synthesized for the first time utilizing pulse laser ablation in liquid method (PLAL). Qswitched neodymium-doped yttrium aluminum garnet (Nd: YAG) laser was used to prepare suspension at different laser fluence in water environment for LN and Au targets, then deposited at n-Type silicon substrates. XRD analysis used to define the structure nature of these films. Photoluminescence measurements exhibited distinct emissions peaks that decreased as the laser fluence escalated. The surface morphology was examined using field emission scanning electron microscopy (FESEM) and transmission electron microscopy (TEM), while image j software was used to determine surface nature and particles size of Au- LiNbO3 thin films. It is found aggregation threshold decrease as laser fluence increases with zeta potential ranging about -16 to -12 mV..