Deposition Temperature and Heat Treatment on Silicon Nitride Coating Deposited by LPCVD

doi:10.15541/jim20190035

Abstract

Abstract:

Silicon nitride coatings on carbon fiber cloth were prepared by Low Pressure Chemical Vapor Deposition (LPCVD) from gas mixtures of SiCl₄-NH₃-H₂ at temperatures ranging from 750 ℃to 1250 ℃. The effects of deposition temperature on the growth kinetics, morphologies, chemical composition and bonding state of the coatings were investigated. The results showed that deposition rate increased monotonously with temperature up to 1050 ℃, then it reversely decreased. In the whole temperature range, the coating surface morphology became gradually coarse with cauliflower-like grains as the deposition temperature increased. The optimal deposition temperature for infiltration was in the range between 750 and 950 ℃. Chemical composition analysis demonstrated that the nitrogen content of the coating firstly decreased and then increased with temperature increase, while the silicon content continuously increased and the oxygen content gradually decreased in the whole temperature range. Heat treatment at 1300 ℃ and above crystallized the coating. Concurrently, a significant change in its surface morphology was observed. All heat-treated coatings were exclusively composed of a-Si₃N₄, without the presence of any b-Si₃N₄.

Key words: silicon nitride coating, growth kinetic, deposition temperature, chemical composition, heat treatment

CLC Number:

TQ174

LIAO Chun-Jing, DONG Shao-Ming, JIN Xi-Hai, HU Jian-Bao, ZHANG Xiang-Yu, WU Hui-Xia. Deposition Temperature and Heat Treatment on Silicon Nitride Coating Deposited by LPCVD[J]. Journal of Inorganic Materials, 2019, 34(11): 1231-1237.

Figures/Tables 8

Fig. 1 Deposition rate as a function of temperature for SiCl4-NH3-H2 system

Fig. 2 Surface morphologies of silicon nitride coatings coated carbon fiber cloth at different temperatures (a, b) Original; (c, d) 750 ℃; (e, f) 950 ℃; (g, h) 1150 ℃

Fig. 3 Fracture morphologies of silicon nitride deposited on the carbon fiber cloth at different temperatures The left figures show outer coating morphologies of carbon fiber cloth while the right figures show their corresponding inner coating morphologies: (a) 750 ℃; (b) 850 ℃; (c) 950 ℃; (d) 1050 ℃; (e) 1150 ℃

Deposition temperature/℃	Elemental type and elemental contents/at%
Deposition temperature/℃	N	Si	O
750	53.21	30.78	16.01
850	46.92	43.25	9.82
950	43.67	43.49	12.84
1050	50.43	43.60	5.97
1150	49.88	46.87	3.24

Fig. 4 N1s and Si2P XPS spectra of silicon nitride coatings deposited at different temperatures (a-b) 750 ℃; (c-d) 950 ℃; (e-f) 1150 ℃; (a, c, e) NIS spectra; (b, d,f) Si2P spectra

Fig. 5 FT-IR spectra of silicon nitride coatings heat-treated at different temperatures (a) As-deposited; (b) 1300 ℃; (b) 1400 ℃; (d) 1500 ℃

Fig. 6 XRD patterns of as-deposited coatings heat-treated at different temperatures (a) 1300 ℃; (b) 1400 ℃; (c) 1500 ℃

Fig. 7 Surface morphology of silicon nitride coating deposited at 850 ℃ followed by heat treatment at 1500 ℃ for 2.5 h in Ar

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