上浆剂对国产T800级碳纤维增强热固性复合材料界面性能的影响

王新庆; 柳肇博; 刘寒松; 肇研; 关志东

doi:10.13801/j.cnki.fhclxb.20220104.001

上浆剂对国产T800级碳纤维增强热固性复合材料界面性能的影响

doi: 10.13801/j.cnki.fhclxb.20220104.001

王新庆^1,,
柳肇博^2,,
刘寒松²,
肇研^{1, 2, ,},
关志东¹

1.
北京航空航天大学　航空科学与工程学院，北京 100191
2.
北京航空航天大学　材料科学与工程学院，北京 100191

详细信息

通讯作者:
肇研，博士，教授，博士生导师，研究方向为先进树脂基复合材料　 E-mail: jennyzhaoyan@buaa.edu.cn

中图分类号: TB332
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出版历程
- 收稿日期: 2021-10-09
- 修回日期: 2021-12-09
- 录用日期: 2021-12-26
- 网络出版日期: 2022-01-04
- 刊出日期: 2022-08-22

Effect of sizing agent on interfacial properties of domestic T800 grade carbon fiber reinforced thermosetting composites

1.
School of Aeronautic Science and Engineering, Beihang University, Beijing 100191, China
2.
School of Materials Science and Engineering, Beihang University, Beijing 100191, China

摘要

摘要: 碳纤维具有力学性能优、密度低、耐腐蚀、耐高温等一系列优异性能，近年来被广泛应用于航空、航天等重要领域。相较于国外的高强中模碳纤维，国内虽有T800级碳纤维与之对应，但是国内对高性能碳纤维的研究工作起步晚，研究尚不充分。上浆剂作为碳纤维表面的重要组成部分，对碳纤维的表面性能有着重要的影响，进而影响复合材料的界面性能。本文采用SEM、TGA、XPS等表征手段，研究分析了上浆剂对国产T800级碳纤维的影响，对碳纤维的表面物化特性及其不同先进树脂基复合材料的微观界面性能进行研究，为国产高性能碳纤维的产品发展提供借鉴意义。
- 碳纤维 /
- 上浆剂 /
- 复合材料 /
- 界面性能 /
- 力学性能
Abstract: Carbon fiber has a series of excellent properties such as low density, high specific strength, high specific modulus, corrosion resistance, high temperature resistance, and good fatigue resistance. In recent years, it has been widely used in important fields such as aviation and aerospace. Compared with the high-strength medium-mold carbon fiber abroad, although there is T800 grade carbon fiber in China, the research work on high-performance carbon fiber in China has started late, and the research is not enough, and the products are not comparable to those in foreign countries. Sizing agent , as an important part of carbon fiber surface, has an important effect on the surface properties of carbon fiber and the interfacial properties of composites. The effect of sizing agent on domestic T800 carbon fiber was studied and analyzed by means of SEM, TGA and XPS. In this work, the surface characteristics of carbon fiber and the microscopic interface of the composite material has been studied, which provide a reference for the development of domestic high-performance carbon fiber products.
- carbon fiber /
- sizing agent /
- composites /
- interface property /
- mechanical property

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图 1 不同碳纤维侧面形貌的的SEM图像：((a), (g)) 800-1；((b), (h)) 800-2；((c), (i)) 800-3；((d), (j)) 800-4；((e), (k)) 800-5；((f), (l)) 800-6

Figure 1. SEM images of carbon fibers surface morphology: ((a), (g)) 800-1; ((b), (h)) 800-2; ((c), (i)) 800-3; ((d), (j)) 800-4; ((e), (k)) 800-5; ((f), (l)) 800-6

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图 2 不同碳纤维断口截面形貌图(×10000倍): (a) 800-1；(b) 800-2；(c) 800-3；(d) 800-4；(e) 800-5；(f) 800-6

Figure 2. SEM images of carbon fibers fracture section(×10000 times): (a) 800-1; (b) 800-2; (c) 800-3; (d) 800-4; (e) 800-5; (f) 800-6

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图 3 上浆剂在N₂中的热重曲线

Figure 3. TG curves of sizing agent in N₂

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图 5 碳纤维表面XPS的C1s拟合峰：(a) 800-1；(b) 800-2；(c) 800-3；(d) 800-4；(e) 800-5；(f) 800-6

Figure 5. XPS C1s spectra of carbon fiber: (a) 800-1; (b) 800-2; (c) 800-3; (d) 800-4; (e) 800-5; (f) 800-6

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图 4 碳纤维表面的XPS全谱扫描分析

Figure 4. XPS spectrum of carbon fiber

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图 6 浸润性能测试示意图：(a) 树脂在碳纤维表面形成的树脂微球；(b) 参数m测量示意图

Figure 6. Infiltration performance test schematic diagram: (a) Resin in the carbon fiber surface resin microspheres; (b) Schematic diagram of parameter m measurement

a—Short axis of the ellipse; b—Long axis of the ellipse

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图 7 碳纤维增强树脂基复合材料的微观界面剪切强度

Figure 7. Interfacial shear strength of carbon fiber reinforced resin matrix composites

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图 8 碳纤维增强树脂基复合材料的微脱粘断面形貌：(a) 800-1/A；(b) 800-1/B；(c) 800-2/A；(d) 800-2/B；(e) 800-3/A；(f) 800-3/B；(g) 800-4/A；(h) 800-4/B；(i) 800-5/A；(j) 800-5/B；(k) 800-6/A；(l) 800-6/B

Figure 8. Interfacial shear strength fracture appearance of carbon fiber reinforced resin matrix composites: (a) 800-1/A; (b) 800-1/B; (c) 800-2/A; (d) 800-2/B; (e) 800-3/A; (f) 800-3/B; (g) 800-4/A; (h) 800-4/B; (i) 800-5/A; (j) 800-5/B; (k) 800-6/A; (l) 800-6/B

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图 9 碳纤维增强树脂基复合材料的断面形貌：((a), (b)) 800/A树脂；((c), (d)) 800/B树脂

Figure 9. Section morphologies of carbon fiber reinforced resin matrix composites: ((a), (b)) 800/A resin; ((c), (d)) 800/B resin

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表 1 碳纤维表面上浆处理

Table 1. Sizing treatment of carbon fiber

Carbon fiber	Molecular weight	Sizing agent content/%
800-1	Low	1.3
800-2	High	1.3
800-3	Low	1.4
800-4	High	1.4
800-5	Low	1.6
800-6	High	1.6

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表 2 六种碳纤维上浆量测试结果

Table 2. Test results of sizing agent content of six kinds of carbon fibers

Carbon fiber	Sizing agent content/%
800-1	1.30
800-2	1.32
800-3	1.36
800-4	1.39
800-5	1.63
800-6	1.63

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表 3 碳纤维表面上浆剂失重5wt%时的热分解温度

Table 3. Thermal decomposition temperature at 5wt% mass loss of carbon fiber surface sizing agent

Sizing agent	5wt% mass thermal decomposition temperature/℃
800-A1	290.2
800-A2	274.5
800-A3	278.2
800-A4	274.2
800-A5	276.6
800-A6	271.1

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表 4 碳纤维表面元素成分及含量

Table 4. Surface element composition and content of carbon fiber

Carbon fiber	C1s 284.8 eV	O1s 532.7 eV	N1s 400.9 eV	S2p 168.6 eV	Si2p 102.3 eV	O/C
800-1	75.37	18.47	1.74	0.40	4.02	0.245
800-2	80.33	16.41	2.85	0.41	0	0.204
800-3	76.19	17.34	2.02	0.56	3.90	0.228
800-4	77.31	16.25	2.28	0	4.15	0.210
800-5	75.67	17.26	1.96	0.62	4.50	0.228
800-6	77.27	16.41	1.96	0.52	3.84	0.212

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表 5 上浆后碳纤维表面XPS的C1s拟合峰结果

Table 5. XPS C1s spectrum of carbon fiber

Carbon fiber	—C—C— or —C—H/% 284.8 eV	—C—OH or —C—OR/% 286.3 eV	—C=O/% 287.8 eV	—COOH or —COOR/% 288.9 eV	Active C/%
800-1	56.85	33.34	1.58	8.23	43.15
800-2	54.15	35.30	0.42	10.13	45.85
800-3	60.63	29.47	1.85	8.05	39.37
800-4	52.57	25.06	11.97	10.40	47.43
800-5	66.09	22.69	3.53	7.69	33.91
800-6	60.64	31.89	0.03	7.44	39.36

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表 6 碳纤维表面的浸润性能测试结果

Table 6. Wetting property test results of carbon fiber surface

Carbon fiber	Parameter m
Carbon fiber	A resin	B resin
800-1	0.724	0.735
800-2	0.721	0.720
800-3	0.715	0.718
800-4	0.736	0.715
800-5	0.719	0.725
800-6	0.739	0.728

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表 7 碳纤维增强复合材料宏观力学性能

Table 7. Macroscopic mechanical properties of carbon fiber reinforced composites

Sample	ILSS/MPa	Flexural strength/MPa
800/A resin	111.75	1800
800/B resin	87.43	1900
Note: ILSS—Interlaminar shear strength.

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