连续玄武岩纤维/环氧树脂复合材料的润湿渗透剂表面改性及其非线性蠕变性能

张颜锋; 朱四荣; 别依诺; 陆士平; 贺攀

doi:10.13801/j.cnki.fhclxb.20230825.002

连续玄武岩纤维/环氧树脂复合材料的润湿渗透剂表面改性及其非线性蠕变性能

doi: 10.13801/j.cnki.fhclxb.20230825.002

1.
武汉理工大学　新材料力学理论与应用湖北省重点实验室，武汉 430070
2.
上海富晨化工有限公司，GB51160国家标准管理组，上海 200241
3.
成都纺织高等专科学校，成都 611731

基金项目: 国家自然科学基金(12202325)

详细信息

通讯作者:
朱四荣，博士，教授，博士生导师，研究方向为复合材料结构设计及复合材料长期力学性能研究　E-mail: zhusirong@whut.edu.cn

中图分类号: TB332
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- 被引次数: 0
出版历程
- 收稿日期: 2023-06-12
- 修回日期: 2023-08-08
- 录用日期: 2023-08-14
- 网络出版日期: 2023-08-28
- 刊出日期: 2024-04-15

Study on the surface modification of wetting penetrant and nonlinear creep of continuous basalt fiber/epoxy resin composites

1.
Hubei Key Laboratory of Theory and Application of Advanced Materials Mechanics, Wuhan University of Technology, Wuhan 430070, China
2.
GB51160 National Standards Management Group, Shanghai Fuchen Chemical CO., LTD., Shanghai 200241, China
3.
Chengdu Textile College, Chengdu 611731, China

Funds: National Natural Science Foundation of China (12202325)

摘要

摘要: 采用润湿渗透剂协同硅烷偶联剂对玄武岩纤维(BF)进行表面改性，并缠绕成型制备了玄武岩纤维/环氧树脂(BF/EP)复合材料。采用万能材料试验机测定了BF/EP的弯曲性能及在不同应力水平下测定了BF/EP复合材料240 min的蠕变性能，借助场发射扫描电子显微镜(FESEM)观察了纤维及弯曲断裂断口的表面形貌，并分析了纤维表面改性对各项力学性能的影响。结果表明：采用润湿渗透剂协同硅烷偶联剂对BF进行表面改性后，BF/EP弯曲性能得到有效改善，层间剪切强度得到提高，FESEM形貌显示BF的协同改性提高了纤维与树脂之间的界面性能；在多种应力水平下的短期蠕变实验中，均表现出蠕变柔量增量的显著降低。使用改进Findley模型可描述BF/EP复合材料在低于其断裂应力水平下的蠕变性能，以此可进行其在不同应力水平下的蠕变性能预测。
- 表面改性 /
- 润湿渗透剂 /
- BF/EP复合材料 /
- 非线性蠕变 /
- 改进Findley模型
Abstract: The surface modification of basalt fiber (BF) was carried out by using a wetting and penetrating agent in conjunction with a silane coupling agent, followed by winding and molding to prepare basalt fiber/epoxy resin (BF/EP) composite materials. The bending performance of BF/EP was determined using a universal material testing machine, and the creep properties of BF/EP composite materials were measured at different stress levels for 240 min. The surface morphology of the fiber and the bending fracture surface were observed by field emission scanning electron microscopy (FESEM), and the effect of fiber surface modification on various mechanical properties was analyzed. The results show that the surface modification of BF using a wetting and penetrating agent in combination with a silane coupling agent is an effective approach to enhance the bending performance and interlaminar shear strength of BF/EP composites. The FESEM morphology analysis reveals that this synergistic modification of BF enhances the interfacial properties between the fiber and the resin, which contributes to the improved mechanical properties of the composite material. Moreover, the short-term creep experiments conducted at various stress levels indicate a significant reduction in creep compliance increment, which suggests that the modified BF/EP composite material has better creep resistance. The improved Findley model provides a useful tool to predict the creep properties of BF/EP composites at different stress levels, which can help optimize their design and performance in practical applications.
- surface modification /
- wetting penetrant /
- basalt fiber/epoxy resin composite material /
- nonlinear creep /
- improving the Findley model

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图 1 壬基酚聚氧乙烯醚的结构

Figure 1. Structure diagram of nonylphenol polyoxyethylene ether

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图 2 润湿渗透剂协同硅烷偶联剂上浆剂对玄武岩纤维(BF)改性效果对比示意图

Figure 2. Comparison diagram of modification effect of wetting penetrant combined with silane coupling agent sizing agent on basalt fiber (BF)

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图 3 BF表面微观形貌

Figure 3. Surface morphology of BF

KH-560-BF—BF modified by KH-560; WA-KH-560/570-BF—BF modified by wetting agent-KH-560/570

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图 4 BF/环氧树脂(EP)复合材料弯曲断口形貌

Figure 4. Morphologies of bending fracture of BF/epoxy resin (EP) composites

KH-560-BF/EP—BF/EP made of BF modified by KH-560;WA-KH-560/570-BF/EP—BF/EP made of BF modified by wetting agent-KH-560/570

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图 5 BF/EP复合材料层间剪切破坏试样

Figure 5. Inter-laminar shear failure samples of BF/EP composites

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图 6 BF/EP复合材料蠕变柔量增量在各应力水平下随时间的变化曲线

Figure 6. Curves of creep compliance increment of BF/EP composites at various stress levels vs time

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图 7 BF/EP复合材料拟合曲线h(σ)

Figure 7. Fitting curves of BF/EP composites h(σ)

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图 8 BF/EP复合材料蠕变模型与试验结果对比

Figure 8. Comparison of creep model and test results of BF/EP composites

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图 9 BF/EP复合材料35%应力水平下预测曲线与试验结果对比

Figure 9. Comparison of prediction curve and test results of BF/EP composites at 35% stress level

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表 1 硅烷偶联剂改性法(对照组)的上浆剂成分

Table 1. Sizing agent composition of silane coupling agent modified method (control group)

Type of reagent	Mass fraction/wt%
Silane coupling agent (KH-560)	0.50
Glacial acetic acid	0.05
Epoxy emulsion	6.00
Film-forming additive	0.30

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表 2 润湿渗透剂/硅烷偶联剂协同改性法的上浆剂成分

Table 2. Sizing agent composition of wetting penetrant/silane coupling agent synergistic modification method

Type of reagent	Mass fraction/wt%
Silane coupling agent (KH-560)	0.30
Silane coupling agent (KH-570)	0.20
Glacial acetic acid	0.08
Epoxy emulsion	6.00
Film-forming additive	0.30
Wetting agent	0.50
Lubricant	0.20

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表 3 BF丝束及其浸胶纱的拉伸性能

Table 3. Tensile properties of BF tow and its resin-impregnated yarn

Sample	P/(N·tex⁻¹)	σ_t/MPa	E_t/GPa
KH-560-BF	0.570	2722.8	89.1
WA-KH-560/570-BF	0.674	2938.2	92.0
Notes: P—Tensile strength of BF bundle; σ_t—Tensile strength of BF resin-impregnated yarn; E_t—Tensile modulus of BF resin-impregnated yarn.

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表 4 BF/EP复合材料弯曲性能

Table 4. Banding property of BF/EP composites

Sample	σ_f /MPa	E_f /GPa
KH-560-BF/EP	837.5	26.6
WA-KH-560/570-BF/EP	1157.0	32.2
Notes: σ_f—Flexural strength; E_f—Flexural modulus.

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表 5 BF/EP复合材料层间剪切强度

Table 5. Inter-laminar shear strength of BF/EP composites

Sample	τ_s/MPa
KH-560-BF/EP	39.0
WA-KH-560/570-BF/EP	49.9
Note: τ_s—Interlaminar shear strength.

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表 6 不同应力水平下BF/EP复合材料的蠕变柔量增量(240 min)

Table 6. Creep compliance increment of BF/EP composites at various stress levels (240 min)

Stress level	Creep compliance increment/(10⁻¹² Pa⁻¹)
Stress level	KH-560-BF/EP	WA-KH-560/570-BF/EP
20%	1.882	0.675
30%	1.842	0.765
40%	2.375	1.210
45%	2.420	1.490
50%	3.140	1.870

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表 7 不同应力水平下h(σ)的拟合值

Table 7. Fitting values of h(σ) at different stress levels

Stress level	h(σ)
Stress level	KH-560-BF/EP	WA-KH-560/570-BF/EP
20%	1	1
30%	1.01	1.18
40%	1.28	1.82
45%	1.32	2.19
50%	1.69	2.71
Note: h(σ)—Functions related to stress level.

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表 8 BF/EP复合材料不同应力水平的拟合优度R²

Table 8. Goodness-of-fit R² of BF/EP composites at different stress levels

Stress level	R²
Stress level	KH-560-BF/EP	WA-KH-560/570-BF/EP
20%	0.998	0.997
30%	0.994	0.994
40%	0.999	0.999
45%	0.997	0.994
50%	0.999	0.988

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表 9 BF/EP复合材料蠕变柔量增量预测值误差(240 min)

Table 9. Predicted value error of creep compliance increment in BF/EP composites (240 min)

Sample	J_t/(10⁻¹³ Pa⁻¹)	J_c/(10⁻¹³ Pa⁻¹)	Deviation/%
KH-560-BF/EP	20.70	20.50	0.90
WA-KH-560/570-BF/EP	9.53	9.74	2.18
Notes: J_t—Experimental value of creep compliance; J_c—Calculated value of creep compliance.

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