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CVD of Silicon Nitride Plate from HsiCl3-NH3-H2 Mixtures

Published online by Cambridge University Press:  15 February 2011

J. W. Lennartz
Affiliation:
Union Carbide Coatings Service Corporation, 12900 Snow Road, Parma, OH 44130
M. B. Dowell
Affiliation:
Union Carbide Coatings Service Corporation, 12900 Snow Road, Parma, OH 44130
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Abstract

Preferred conditions for deposition of thick α-Si3 N4 plate from HSiCl3 -NH3-H2 on the vertical surfaces of a lowpressure, hot-wall CVD reactor were identified by means of a designed experiment. The design included the range of temperatures 1300°C-1500°C, pressures 0.5–2.0 Torr, and residence times 0.01–1.0 sec. The vertical deposition surfaces received a viscous, laminar flow of well mixed, thermally equilibrated reactants. Plates 0.05–0.5 mm thick were produced on multiple vertical substrates 350 cm2 in area at deposition rates 5–70 μm/hr. Plates 0.5–4.0 mm thick were produced on horizontal substrates at deposition rates of 60–120 μm/hr. When NH3 flows in stoichiometric excess, deposition rates on vertical surfaces increase approximately linearly with the flow rate of HSiCl3 but depend little on temperature, as would be expected if the reaction proceeds under mass transport control with product depletion. Multiple correlation analyses show that thickness variations in the deposit are reduced by increasing the temperature and decreasing the gas residence time. CVD silicon nitride plate produced under the optimized conditions exhibits theoretical density and is free of pores and cracks. It exhibits a columnar morphology in which the <222> and <101> crystallographic directions are oriented preferentially normal to a surface, which consists of well-defined trigonal facets 10–50 μm across. Crystallite sizes determined by Xray line broadening range from 0.06–1.0 μm. This CVD plate is gray and contains approximately 0.5 w/o C and 0.5 w/o 0 as principal impurities.

Type
Research Article
Copyright
Copyright © Materials Research Society 1992

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