Boron carbide was prepared by low pressure chemical vapor deposition (LPCVD) from BCl3-CH4-H-2 system. The deposition process conditions were optimized through using a uniform design method and regression analysis. The regression model of the deposition rate was established. The influences of deposition temperature (T), deposition time (t), inlet BCl3/CH4 gas ratio (delta), and inlet H-2/CH4 gas ratio (theta) on deposition rate and microstructure of the coatings were investigated. The optimized deposition parameters were obtained theoretically. The morphologies, phases, microstructure and composition of deposits were characterized using scanning electron microscopy (SEM), X-ray diffraction (XRD), Raman micro-spectroscopy, transmission electron microscopy (TEM), energy dispersive spectra (EDS), and Auger electron spectra (AES), the results showed that different boron carbides were produced by three kinds of deposition mechanisms. Crown Copyright (C) 2009 Published by Elsevier B.V. All rights reserved.