碳纤维复合Si3N4陶瓷材料的制备及性能研究

doi:10.15541/jim20140165

摘要/Abstract

摘要：

为研究碳纤维(C_f)加入量对复合材料性能的影响, 本研究以Y₂O₃为烧结助剂, 采用热压烧结技术制备了C_f/Si₃N₄复合材料, 其中碳纤维加入量为0、2wt%和5wt%。选用乙醇作分散介质,通过球磨工艺可有效分散短切碳纤维。研究结果表明: 碳纤维在复合材料中分散均匀, 且材料中的晶粒在垂直于热压压力的方向呈现一定取向排列。高温烧结过程中, 碳纤维与Si₃N₄或其表面的SiO₂层发生反应, 生成SiC中间层。适量碳纤维加入有助于提高复合材料的热导性能。当C_f加入量为2wt%时,C_f/Si₃N₄的热导率较高, 为45.8 W/(m?K);而不添加C_f的样品, 其热导率为37.1 W/(m?K)。加入C_f后, C_f/Si₃N₄的断裂韧性有小幅提高, 维氏硬度在16.6~16.8 GPa范围内变化。

关键词: C_f/Si₃N₄复合材料, 热压烧结, 界面反应, 热导, 力学性能

Abstract:

To investigate the effects of carbon fiber (C_f) adding content on the properties of Si₃N₄, C_f/Si₃N₄ composites with 0, 2wt% and 5wt% of short carbon fibers were prepared by hot-press sintering method, using Y₂O₃as sintering additives_. With long-time ball milling process, carbon fibers were well dispersed in mixed powders using ethanol as dispersion medium. Carbon fibers distribute uniformly in the composites and Si₃N₄grains grow to a certain degree in the vertical direction to the pressure of hot-press. The interfacial by-product silicon carbide (SiC) phase forms due to the reaction between added C_f and Si₃N₄ particles or SiO₂ layer on surface of Si₃N₄ particles during high temperature sintering. The sample with 2wt% C_f addition achieves a higher value of thermal conductivity (45.8 W/(m?K)), while the thermal conductivity of Si₃N₄without C_f is only 37.1 W/(m?K). Therefore, the addition of C_f can improve the thermal conductivity of the composites. The fracture toughness of the composites has a slight increase with C_f adding. The measured hardness values for all samples are within a range of 16.6-16.8 GPa.

Key words: Cf/Si3N4 composite, hot-press sintering, interfacial reaction, thermal conductivity, mechanical property

王贺云, 刘茜, 周遥, 周真真，刘光辉. 碳纤维复合Si₃N₄陶瓷材料的制备及性能研究[J]. 无机材料学报, 2014, 29(9): 1003-1008.

WANG He-Yun, LIU Qian, ZHOU Yao, ZHOU Zhen-Zhen, LIU Guang-Hui. Preparation and Properties of Carbon Fiber/Si₃N₄ Composites[J]. Journal of Inorganic Materials, 2014, 29(9): 1003-1008.

图/表 8

Fig. 1 SEM images of raw Si3N4 particles (a) and raw carbon fibers (b)

Fig. 2 XRD patterns of raw Si3N4 powders and Cf/Si3N4 composites

Fig. 3 SEM and optical microscopy images of Cf/Si3N4 Secondary electron image (SEI) of fracture surfaces of SN-Cf-0 (a) and SN-Cf-5 (b), back scattered electron image (BSEI) of fracture surface of SN-Cf-5 (c), and optical microscopy image of SN-Cf-5 surface (d)

Fig. 4 TEM image of interfacial surface between Cf and Si3N4 in SN-Cf-5 (a) and EDS patterns of different regions (b, c, d) arrowed in (a)

Fig. 5 TEM (a) and HRTEM (b) images of interfacial transition layer of SiC in SN-Cf-5 specimen

Table 1 Thermal properties of Cf/Si3N4 composites measured at room temperature

Composites	C_f/ wt%	ρ/ (g?cm^-3)	C_p/ (mm²?s^-1)	α/ (J?g^-1?K^-1)	k/ (W?m^-1?K^-1）
SN-Cf-0	0	3.27	17.98	0.59	37.12
SN-Cf-2	2	3.31	19.99	0.61	45.84
SN-Cf-5	5	3.28	15.12	0.58	33.43

Fig. 6 Variation of thermal conductivity with temperature for Cf/Si3N4 composites

Table 2 Mechanical property of Cf/Si3N4 composites measured at room temperature

Composites	C_f/wt%	H_v/GPa	K_IC/(MPa?m^1/2)
SN-Cf-0	0	16.6	5.0
SN-Cf-2	2	16.8	4.9
SN-Cf-5	5	16.8	5.3

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碳纤维复合Si₃N₄陶瓷材料的制备及性能研究

Preparation and Properties of Carbon Fiber/Si₃N₄ Composites

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