Chromium carbide coatings were grown at 748 K in a hot wall CVD reactor fed by sublimation of bis(benzene)chromium, BBC (MOCVD) and by direct liquid injection using a BBC/toluene solution (DLICVD). The two types of coatings exhibit an amorphous structure and the same C content (22 at.%). DLICVD permits delivering higher mass flow rate of precursors and consequently the growth rate is 3 times higher and the thickness uniformity is better than using MOCVD. Chromium metal deposition has also been investigated by DLICVD in this hot wall reactor using BBC/toluene/additive as precursor. The purpose of the additive is to block carbide formation. Two additives have been studied: (i) hexachlorobenzene (C6Cl6) and (ii) thiophenol (C6H5SH). The ratio additive/BBC required for Cr metal deposition is a few percent. In this process, C6Cl6 is not decomposed and only traces of Cl (0.4 at.%) are found in the coatings. For a ratio C6Cl6/BBC > 27% the growth of any coating is blocked. The gas phase containing C6H5SH is more reactive since the onset of deposition occurs approximately 50 K before the temperature of the chlorinated compound. Furthermore, a sulfur contamination of 3 at.% has been analyzed in the coatings revealing a partial decomposition of the additive. The results are detailed and discussed in relation with previous works.
Frédéric Schuster. SiC coatings grown by liquid injection chemical vapor deposition using single source metal-organic precursors. Surface and Coatings Technology, Elsevier, 2013, vol. 215, pp. 152-160. 10.1016/j.surfcoat.2012 SiC coatings have been grown by direct liquid injection of organosilanes in a hot-wall chemical vapor deposition reactor (DLICVD). 1,3-disilabutane (DSB) and polysilaethylene (PSE) were used as single-source precursors. Amorphous and stoichiometric SiC coatings were deposited under low pressure on various substrates in the temperature range of 923-1073 K. Thickness gradients due to the temperature profiles and the precursor depletion were observed along the reactor axis but the thickness uniformity could be improved as a function of the deposition conditions. Growth rates as high as 90 μm·h −1 were obtained using pure precursors. The injection of PSE solutions in toluene significantly reduces the deposition rate due to the decrease of the PSE mole fraction but allows a better control of the growth rates and the microstructure of coatings. They exhibit a smooth surface morphology and a very dense structure. The films grown using pure precursors exhibit an Si:C atomic ratio equal to 1:1 while those using toluene solutions are slightly C-rich (54 at.% C). The presence of solvent vapor in the CVD reactor becomes a source of carbon contamination at deposition temperatures equal to or higher than 1073 K. The influence of the growth conditions is discussed, in particular the presence of toluene vapor.
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