不同先驱体制备C/SiC复合材料及其浸渍行为

doi:10.15541/jim20190541

摘要/Abstract

摘要：

采用先驱体浸渍裂解工艺(PIP工艺)制备C/SiC复合材料, 研究了不同先驱体对复合材料浸渍行为的影响(三种先驱体分别为固态聚碳硅烷(PCS(s))、液态聚碳硅烷Ⅰ(PCS-Ⅰ(l))和液态聚碳硅烷Ⅱ(PCS-Ⅱ(l)), 制备的三种复合材料体系分别为C/SiC-0、C/SiC-Ⅰ和C/SiC-Ⅱ)。结合C/SiC复合材料的力学性能以及不同裂解周期C/SiC复合材料的微观形貌, 研究了不同先驱体制备的C/SiC复合材料对碳纤维织物浸渍行为的影响。研究结果表明: C/SiC-Ⅰ复合材料的室温弯曲强度最高, 达到336 MPa。不同裂解周期的微观形貌显示, C/SiC-0复合材料内部孔隙分布于碳纤维束间; C/SiC-Ⅰ复合材料内部较致密, 孔隙分布均匀; C/SiC-Ⅱ复合材料基体和束丝内部都存在孔隙, 说明三种聚碳硅烷浸渍液对C/SiC复合材料有不同的浸渍效果。凝胶渗透色谱(GPC)的分析结果显示, 由于浸渍液的分子量不同, 大分子无法浸渍到碳纤维束丝内部, 会造成裂解后的复合材料束内SiC基体较少, 造成其力学性能较低。

关键词: 浸渍, 固态聚碳硅烷, 液态聚碳硅烷, C/SiC复合材料

Abstract:

In order to investigate the influence of precursors on impregnation behaviors of C/SiC composites, C/SiC composites (C/SiC-0,C/SiC-Ⅰand C/SiC-Ⅱ) prepared with three different precursors (solid polycarbosilane, PCS(s)), liquid polycarbosilane PCS-Ⅰ(l) and PCS-Ⅱ(l)) were prepared via precursor infiltration and pyrolysis (PIP) method. Impregnation behaviors of different precursors were studied to mainly focuse on the combination of mechanical properties as well as microstructures of C/SiC composites with different PIP cycles. Results showed that C/SiC-Ⅰ composites exhibited the highest flexural strength of 336 MPa. The microstructures of C/SiC composites showed that the internal pores of C/SiC-0 composites were distributed between carbon fiber bundles, C/SiC-I composites were dense and the pores were evenly distributed. The pores of C/SiC-II composites were inside carbon fiber bundles and SiC matrix. Gel permeation chromatography (GPC) results showed that due to the difference of molecular weights of the impregnating solution, the macromolecules cannot impregnated into the carbon fiber bundles, which resulted in the lack of SiC matrix and degradation of mechanical properties for the composites after PIP cycles.

Key words: impregnation, solid polycarbosilane, liquid polycarbosilane, C/SiC composites

中图分类号:

TB332

张冰玉,王岭,王晓猛,邱海鹏. 不同先驱体制备C/SiC复合材料及其浸渍行为[J]. 无机材料学报, 2020, 35(9): 1017-1022.

ZHANG Bingyu,WANG ling,WANG Xiaomeng,QIU Haipeng. Effect of Precursors on Impregnation Behaviors of C/SiC Composites[J]. Journal of Inorganic Materials, 2020, 35(9): 1017-1022.

图/表 9

表1 不同先驱体制备C/SiC复合材料的密度和孔隙率

Table 1 Density and porosity of C/SiC composites prepared with different precursors

C/SiC composites	Precursors type	Density /(g·cm^-3)	Porosity/%
C/SiC-0	PCS(s)	1.99	5.18
C/SiC-Ⅰ	PCS-Ⅰ(l)	1.98	5.34
C/SiC-Ⅱ	PCS-Ⅱ(l)	1.81	6.12

表2 不同聚碳硅烷先驱体浸渍液分子量

Table 2 Molecular mass of different precursors

Precursors type	mn	mw	mp	mz
PCS(s)	1698	4813	6221	10951
PCS-Ⅰ(l)	1077	4051	2211	14695
PCS-Ⅱ(l)	4495	5735	3369	8010

图1 惰性气氛保护下, 先驱体聚碳硅烷的TGA曲线

Fig. 1 TGA curves of PCS pyrolysis in inert atmosphere

表3 不同先驱体制备的C/SiC复合材料室温弯曲强度和弯曲模量

Table 3 Flexural strength and modulus of C/SiC composites prepared with different precursors

Specimen	Average flexural strength/MPa	Average flexural modulus/GPa
C/SiC-0	293	49.1
C/SiC-Ⅰ	336	53.8
C/SiC-Ⅱ	280	47.1

图2 不同先驱体制备的C/SiC复合材料室温弯曲应力-应变曲线

Fig. 2 Flexural strain-stress curves of C/SiC composites with different precursors

图3 C/SiC复合材料首周期裂解后的SEM照片

Fig. 3 SEM images of C/SiC composites after 1st cycle of PIP process (a) C/SiC-0; (b) C/SiC-Ⅰ; (c) C/SiC-Ⅱ. Insets are the corresponding enlarged images

图4 C/SiC复合材料第三周期裂解后的SEM照片

Fig. 4 SEM images of C/SiC composites after 3nd cycle of PIP process (a) C/SiC-0; (b) C/SiC-Ⅰ; (c) C/SiC-Ⅱ

图5 C/SiC复合材料第十周期裂解后的SEM照片

Fig. 5 SEM images of C/SiC composites after 10th cycle of PIP process (a) C/SiC-0; (b) C/SiC-Ⅰ; (c) C/SiC-Ⅱ. Insets are the corresponding enlarged images

图6 浸渍液填充碳纤维预制体示意图

Fig. 6 Schematic diagram of impregnation of C fiber preforms

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