A novel fluoro contain polymethylsilsesquioxane (FPMSSQ) nanoparticle has been synthesized by methyltrimethoxysilane(MTMS), tetraethoxysilane(TEOS) and fluorosilane with sol-gel process.The structure characterization of the nanoparticle were conducted by Fourier transform infrared (FT-IR), Differential Scanning Calorimeter (DSC), XRD and Nuclear Magnetic Resonance(NMR).The molecular weight and polydispersity index (PDI) were determined by gel permeation chromatography (GPC).