Effects of heat treatment on the microstructure of amorphous boron carbide coating deposited on graphite substrates by chemical vapor deposition

A two-layer boron carbide coating is deposited on a graphite substrate by chemical vapor deposition from a CH4/BCl3/H-2 precursor mixture at a low temperature of 950 degrees C and a reduced pressure of 10 KPa. Coated substrates are annealed at 1600 degrees C, 1700 degrees C, 1800 degrees C, 1900 degrees C and 2000 degrees C in high purity argon for 2 h, respectively. Structural evolution of the coatings is explored by electron microscopy and spectroscopy. Results demonstrate that the as-deposited coating is composed of pyrolytic carbon and amorphous boron carbide. A composition gradient of B and C is induced in each deposition. After annealing, B4C crystallites precipitate out of the amorphous boron carbide and grow to several hundreds nanometers by receiving B and C from boron-doped pyrolytic carbon. Energy-dispersive spectroscopy proves that the crystallization is controlled by element diffusion activated by high temperature annealing, after that a larger concentration gradient of B and C is induced in the coating. Quantified Raman spectrum identifies a graphitization enhancement of pyrolytic carbon. Transmission electron microscopy exhibits an epitaxial growth of B4C at layer/layer interface of the annealed coatings. Mechanism concerning the structural evolution on the basis of the experimental results is proposed. (C) 2010 Elsevier B.V. All rights reserved.National Natural Science Foundation of China [50532010, 90405015