[Show abstract][Hide abstract] ABSTRACT: 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]
[Show abstract][Hide abstract] ABSTRACT: Amorphous boron carbide (α-B4C) coatings were prepared on SiC substrates by chemical vapor deposition (CVD) from CH4/BCl3/H2/Ar mixtures at low temperature (900–1050 °C) and reduced pressure (10 kPa). The deposited coatings were characterized using scanning electron microscopy (SEM), X-ray diffraction (XRD), micro-Raman spectroscopy, energy dispersive X-ray spectroscopy (EDS) and X-ray photoelectron spectroscopy (XPS). The results showed that two kinds of α-B4C coatings were deposited with different microstructures and phase compositions, and the effect of deposition temperature was significant. When deposited at 1000 °C and 1050 °C, the coatings exhibited a nodular morphology and had a relatively low content of boron. The free carbon was distributed in them inhomogeneously; in contrast, when deposited at 900 °C and 950 °C, the coatings presented a comparatively flat morphology and had a uniform internal structure and high boron content. They did not contain free carbon. At the last of this paper, the pertinent mechanisms resulting in differences in microstructure and phase composition were discussed.
[Show abstract][Hide abstract] ABSTRACT: Boron carbide was prepared by low pressure chemical vapor deposition (LPCVD) from BCl3–CH4–H2 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 (δ), and inlet H2/CH4 gas ratio (θ) 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.