原位生长的气相生长碳纤维增强C/C复合材料的制备及其弯曲性能

doi:10.15541/jim20180058

摘要/Abstract

摘要：

以丙烯为碳源, FeCl₃·6H₂O为催化剂, 采用化学气相沉积法(CVD)在碳毡和不同密度的C/C复合材料上原位气相生长碳纤维(VGCFs) , 并以含原位生长VGCFs的碳毡和不同密度的C/C复合材料为基体制备VGCFs-C/C复合材料。研究了反应压力、基体密度对VGCFs生长情况的影响, 借助扫描电镜(SEM)、光学显微镜观察原位生长VGCFs的形貌及基体原位生长VGCFs后热解炭形貌的变化, 并对比研究了C/C复合材料和VGCFs-C/C复合材料的弯曲性能。研究结果表明, 反应压力为3700 Pa, 基体密度低的情况更有利于VGCFs的生长; 原位生长的VGCFs改变了纤维表面热解炭的沉积形貌, 使得热解炭和碳纤维的结合面之间形成具有铆钉作用的球状结构, 增强了界面结合力, 从而提高了原位生长的高VGCFs含量样品的弯曲强度。

关键词: 气相生长碳纤维, 碳/碳复合材料, 原位生长, 弯曲性能

Abstract:

The in-situ vapor grown carbon fibers (VGCFs) were synthesized by chemical vapor deposition (CVD) on carbon felt and C/C composites of different densities, using propylene as carbon resources and FeCl₃·6H₂O as catalyst. And VGCFs-C/C composites were prepared on carbon felt and C/C composites of different densities with in-situ VGCFs. The effects of pressure in the reactor and density of the substrate on growth of VGCFs were investigated, and the morphology of in-situ VGCFs and the change of morphology of pyrolytic carbon on the substrate with in-situ VGCFs were observed by scanning electron microscope (SEM) and optical microscope. In addition, the flexural properties of C/C composites and VGCFs-C/C composites were investigated. Results show that low density of substrate is beneficial to the in-situ growth of VGCFs when the pressure in the reactor is 3700 Pa. In-situ VGCFs change the morphology of pyrolytic carbon, and induce the formation of the spherical structure, which can enhance the interface bonding force like nails doing. Therefore, the flexural strength of sample with high content of VGCFs is improved.

Key words: vapor grown carbon fibers, C/C composites, in-situ growth, flexural property

中图分类号:

TB332

闫明洋, 杨敏, 李红, 任慕苏, 俞鸣明, 孙晋良. 原位生长的气相生长碳纤维增强C/C复合材料的制备及其弯曲性能[J]. 无机材料学报, 2018, 33(11): 1161-1166.

YAN Ming-Yang, YANG Min, LI Hong, REN Mu-Su, YU Ming-Ming, SUN Jin-Liang. Preparation and Flexural Property of In-situ Vapor Grown Carbon Fibers Reinforced C/C Composites[J]. Journal of Inorganic Materials, 2018, 33(11): 1161-1166.

图/表 14

图1 CVD实验的升温曲线

Fig. 1 The temporal profile of the temperature of CVD experiment

图2 不同压力下碳毡上原位生长VGCFs的形貌

Fig. 2 Morphologies of VGCFs grown in-situ on carbon felt at different pressures

表1 不同压力下碳毡上原位生长VGCFs的质量

Table 1 Mass of VGCFs grown in-situ on carbon felt at different pressures

Pressure/Pa	m₁/g	m₂/g	Δm₁/g
3500	8.7349	8.7873	0.0524
3700	9.5651	10.5503	0.9852
3900	9.1462	9.5761	0.4299

图3 不同密度C/C复合材料基体上原位生长VGCFs的形貌

Fig. 3 Morphologies of VGCFs grown in-situ on C/C composite of different densities

表2 不同密度C/C复合材料基体上原位生长VGCFs的质量

Table 2 Mass of VGCFs grown in-situ on C/C composites of different densities

Density/(g·cm^-3)	m₃/g	m₄/g	Δm₂/g
0.3	551.8821	558.5047	6.6226
0.8	392.5014	395.2516	2.7475
1.3	238.7232	238.7948	0.0716
1.7	209.0905	209.0989	0.0084

图4 加载催化剂后不同密度的基体C/C复合材料的SEM照片

Fig. 4 SEM images of C/C composites of different densities loaded with catalyst

图5 C/C复合材料(A1)与碳毡基体不同反应压力下制备的VGCFs-C/C复合材料(A2~A4)的弯曲应力-应变曲线

Fig. 5 Flexural stress-strain curves of C/C composites (A1) and VGCFs-C/C composites prepared on carbon felt at different pressures (A2-A4)

表3 C/C复合材料(A1)和不同压力下碳毡基体上制备的VGCFs-C/C复合材料(A2~A4)的弯曲性能

Table 3 Flexural properties of C/C composites (A1) and VGCFs-C/C composites prepared on carbon felt at different pressures (A2-A4)

Sample	Density/ (g·cm^-3)	E_f/GPa	σ_f/MPa	CV_Ef/%	CVσ_f/%
A1	1.82	17.14	74.11	4.4	13.2
A2	1.79	27.19	96.93	11.1	10.9
A3	1.80	38.47	142.61	1.9	5.2
A4	1.79	31.37	113.79	4.4	5.6

图6 C/C复合材料和不同压力下碳毡基体上制备的VGCFs-C/C复合材料断口的SEM照片

Fig. 6 Fracture SEM images of C/C composites and VGCFs- C/C composites prepared on carbon felt at different pressures

图7 热解炭在碳纤维上的沉积形貌(a)和热解炭在原位生长VGCFs后碳纤维上的沉积形貌(b)

Fig. 7 Morphologies of pyrolytic carbon on carbon fibers (a) and pyrolytic carbon on carbon fibers with VGCFs (b)

图8 样品A3 (3700 Pa)断口形貌高倍SEM照片

Fig. 8 High magnification fracture SEM morphology of sample A3 (3700 Pa)

图9 不同密度C/C复合材料基体上制备的VGCFs-C/C复合材料的弯曲应力-应变曲线

Fig. 9 Flexural stress-strain curves of VGCFs-C/C composites prepared on C/C composites of different densities

表4 C/C复合材料(A1)和不同密度C/C复合材料制备的VGCFs-C/C复合材料(B1~B4)的弯曲性能

Table 4 Flexural properties of C/C composites (A1) and VGCFs-C/C composites prepared on C/C composites of different densities (B1-B4)

Sample	Density/(g·cm^-3)	E_f/GPa	σ_f/MPa	CV_E_f/%	CVσ_f/%
A1	1.82	17.14	74.11	4.4	13.2
B1	1.81	18.65	105.56	1.9	5.5
B2	1.80	17.92	91.28	6.6	7.2
B3	1.79	11.71	85.03	4.9	12.7
B4	1.82	13.11	84.35	6.5	10.1

图10 不同密度C/C复合材料基体制备的VGCFs-C/C复合材料断口的SEM照片

Fig. 10 Fracture SEM images of VGCFs-C/C composites based on C/C composites of different densities

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