Physicochemical characterizations of polysilicon thin multilayer films have been studied after annealing. In-situ heavily boron-doped polysilicon (poly=Si) and nitrogen-doped silicon (NIDOS) films were deposited by low-pressure chemical vapor deposition (LPCVD) onto an oxidized monocrystalline silicon substrate. Secondary ion mass spectrometry (SIMS) profiles showed a boron diffusion reduction in the NIDOS layer. In addition, Fourier transform infrared spectroscopy (FTIR) analysis clearly showed an evolution of the absorption picks related to the nitrogen atom in the complex form leading to boron atom activation in the films. Therefore, this multilayer structure can be largely used for metal-oxide-semiconductor (MOS) devices.