The aim of this study was to characterize phospholipids bilayers deposited through Langmuir-Blodgett (LB) using Fourier Transform Infrared Spectroscopy (FTIR) and Quartz Crystal Microbalance (QCM) sensor. Phospholipids dimyristoylphosphatidylcholine (DMPC), dimyristoylphosphatidylethanolamine (DMPE), dipalmitoylphosphatidylethanolamine (DPPE) bilayers were deposited. Also, hybrid monolayer of DMPC/Cholesterol (DMPC/CHOL) was prepared. Phospholipid with concentration of 1 mg.ml-1 in chloroform solution was spread at the air-water interface of a Teflon-made LB trough containing a subphase of Milli-Q water using the single-shot method. Phospholipid monolayers were transferred onto the QCM crystal and ZnSe crystals as planar solid support for FTIR measurements using the vertical dipping method. Homogeneous molecular LB films of DMPC, DMPE, DPPE phospholipids and DMPC/CHOL hybrid were produced and characterized by isotherms (Π-area), transfer ratio (θ) and QCM frequency changes results. Also, FTIR spectra results have also indicated the surface molecular organization and packing with the presence of major vibration bands.